Local and long-range order in ferroelastic lead phosphate at high pressure

Pure lead phosphate, Pb₃(PO₄)₂, undergoes a phase transition from C2/c to Rm symmetry at a pressure of approximately 1.8 GPa and room temperature. Single-crystal X-ray diffraction measurements of the unit-cell parameters of a sample doped with 1.6% Ba²⁺ for the Pb²⁺ indicates that the doping reduces the transition pressure by approximately 0.1 GPa. The structural evolution of both samples through the phase transition has been determined by Rietveld refinement of neutron powder diffraction data collected to pressures of 6.3 and 3.3 GPa, respectively. There is no evidence for any significant change in the local structure at the phase transition at high pressures; the structure of the Rm phase at pressures just above the phase transition includes disordered positions for several atoms. The observation of diffuse scattering from the Rm phase at high pressure by single-crystal X-ray diffraction suggests that the disorder is static and arises from the presence of several orientations of the ordered microdomains of the monoclinic local structure. The macroscopic transition from monoclinic to trigonal symmetry therefore appears to correspond to the pressure at which the coherency strains between the locally monoclinic microdomains are sufficient to create a dimensionally trigonal lattice within which local displacements of atoms are still significant. A further pressure increase then decreases the magnitude of these displacements until at 3.5 GPa or higher they are not detectable by our current experimental probes, and the structure appears to have true local and global trigonal symmetry.

Computing details

Data collection: Standard ISIS instrument control program. for S2P0_PEARL. Data reduction: GSAS and in-house data focussing routines. for S2P0_PEARL. Program(s) used to refine structure: GSAS for S2P0_PEARL.

Figures

(S2P0_PEARL)

Crystal data

O8P2Pb3	V = 722.66 Å^3
Mr = 801.86	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7990 (6) Å	T = 298 K
b = 5.6915 (2) Å	Particle morphology: plate
c = 9.4197 (4) Å	irregular, 6 × 6 mm
β = 102.356 (4)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.042	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 108.0 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 5.56 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.042	43 parameters
Rexp = 0.044	10 restraints
R(F^2) = 0.06806	(Δ/σ)max = 0.01
χ^2 = 0.941	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.428488 2: -4.045160E-02 3: 0.235985 4: -0.150751 5: 0.149547 6: -0.139323 7: 8.775510E-02 8: -7.942940E-02 9: 5.115850E-0210: -3.997210E-0211: 8.302940E-0412: -1.521870E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00133 h= 1.000 k= 0.000 l= 0.000 Prefered orientation correction range: Min= 0.99605, Max= 1.00198

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
PB1	0.0	0.2815 (10)	0.25	0.0152 (10)*
PB2	0.3176 (2)	0.3090 (6)	0.3492 (4)	0.0152 (10)*
P	0.60001 (16)	0.2518 (6)	0.4462 (3)	0.0156 (14)*
O21	0.6442 (3)	0.0268 (9)	0.3901 (5)	0.0111 (9)*
O22	0.6290 (3)	0.4696 (10)	0.3665 (5)	0.0111 (9)*
O23	0.6418 (3)	0.2787 (8)	0.6135 (4)	0.0111 (9)*
O1	0.4897 (3)	0.2314 (9)	0.4176 (5)	0.0111 (9)*

Geometric parameters (Å, º)

PB1—PB2	4.284 (3)	O21—PB2^x	2.907 (7)
PB1—PB2^i	4.284 (3)	O21—PB2^xi	3.067 (6)
PB1—PB2^ii	3.930 (6)	O21—PB2^xii	4.477 (5)
PB1—PB2^iii	4.151 (6)	O21—PB2^viii	2.794 (6)
PB1—PB2^iv	3.930 (6)	O21—P^xx	4.499 (5)
PB1—PB2^v	4.151 (6)	O21—P	1.558 (6)
PB1—PB2^vi	4.098 (3)	O21—P^x	4.296 (6)
PB1—PB2^vii	4.098 (3)	O21—P^xi	4.297 (7)
PB1—P^ii	3.649 (5)	O21—P^xviii	4.392 (5)
PB1—P^iii	3.375 (5)	O21—P^xiv	3.755 (6)
PB1—P^iv	3.649 (5)	O21—O21^x	4.278 (9)
PB1—P^v	3.375 (5)	O21—O21^xxi	4.490 (10)
PB1—P^vi	3.438 (3)	O21—O21^xiv	4.084 (10)
PB1—P^vii	3.438 (3)	O21—O22^xx	3.183 (6)
PB1—O21^iii	2.555 (5)	O21—O22	2.534 (6)
PB1—O21^v	2.555 (5)	O21—O22^xxii	4.357 (5)
PB1—O21^vi	4.418 (5)	O21—O22^xiv	3.462 (6)
PB1—O21^vii	4.418 (5)	O21—O23	2.552 (6)
PB1—O22^ii	2.586 (7)	O21—O23^xi	4.306 (7)
PB1—O22^iii	4.344 (8)	O21—O23^xviii	3.128 (7)
PB1—O22^iv	2.586 (7)	O21—O23^xiv	3.161 (7)
PB1—O22^v	4.344 (8)	O21—O1	2.491 (6)
PB1—O23^vi	2.584 (5)	O21—O1^x	3.298 (6)
PB1—O23^vii	2.584 (5)	O21—O1^xi	3.206 (7)
PB1—O1^ii	3.523 (7)	O22—PB1^viii	4.344 (8)
PB1—O1^iii	3.028 (7)	O22—PB1^ix	2.586 (7)
PB1—O1^iv	3.523 (7)	O22—PB2	4.362 (5)
PB1—O1^v	3.028 (7)	O22—PB2^x	2.479 (6)
PB1—O1^vi	3.105 (5)	O22—PB2^xii	2.909 (6)
PB1—O1^vii	3.105 (5)	O22—PB2^ix	3.273 (5)
PB2—PB1	4.284 (3)	O22—P	1.545 (6)
PB2—PB1^viii	4.151 (6)	O22—P^x	4.027 (6)
PB2—PB1^ix	3.930 (6)	O22—P^xii	4.243 (7)
PB2—PB1^vi	4.098 (3)	O22—P^xix	4.204 (5)
PB2—PB2^iv	3.685 (4)	O22—P^xiv	3.982 (6)
PB2—PB2^v	3.685 (4)	O22—O21	2.534 (6)
PB2—PB2^vi	3.778 (7)	O22—O21^xv	3.183 (6)
PB2—P	3.822 (4)	O22—O21^xxiii	4.357 (5)
PB2—P^x	3.239 (5)	O22—O21^xiv	3.462 (6)
PB2—P^xi	3.776 (5)	O22—O22^x	3.761 (9)
PB2—P^xii	3.212 (5)	O22—O22^xiv	4.487 (10)
PB2—P^iii	4.168 (5)	O22—O23	2.539 (6)
PB2—P^vii	4.321 (4)	O22—O23^xii	4.044 (7)
PB2—O21^x	2.907 (7)	O22—O23^xix	2.818 (7)
PB2—O21^xi	3.067 (6)	O22—O23^xiv	3.432 (7)
PB2—O21^xii	4.477 (5)	O22—O1	2.483 (6)
PB2—O21^iii	2.794 (6)	O22—O1^x	3.131 (5)
PB2—O22	4.362 (5)	O22—O1^xii	3.338 (7)
PB2—O22^x	2.479 (6)	O23—PB1^vi	2.584 (5)
PB2—O22^xii	2.909 (6)	O23—PB2^xi	3.398 (6)
PB2—O22^ii	3.273 (5)	O23—PB2^xii	2.420 (6)
PB2—O23^xi	3.398 (6)	O23—PB2^xiii	2.959 (5)
PB2—O23^xii	2.420 (6)	O23—P	1.566 (5)
PB2—O23^vii	2.959 (5)	O23—P^xi	4.446 (7)
PB2—O1	2.365 (5)	O23—P^xii	4.217 (7)
PB2—O1^x	4.055 (6)	O23—P^xvi	4.477 (6)
PB2—O1^xi	4.343 (5)	O23—P^xvii	4.250 (6)
PB2—O1^xii	4.030 (6)	O23—P^xiv	3.728 (6)
P—PB1^viii	3.375 (5)	O23—O21	2.552 (6)
P—PB1^ix	3.649 (5)	O23—O21^xi	4.306 (7)
P—PB1^vi	3.438 (3)	O23—O21^xvi	3.128 (7)
P—PB2	3.822 (4)	O23—O21^xiv	3.161 (7)
P—PB2^x	3.239 (5)	O23—O22	2.539 (6)
P—PB2^xi	3.776 (5)	O23—O22^xii	4.044 (7)
P—PB2^xii	3.212 (5)	O23—O22^xvii	2.818 (7)
P—PB2^viii	4.168 (5)	O23—O22^xiv	3.432 (7)
P—PB2^xiii	4.321 (4)	O23—O23^xiv	4.041 (10)
P—P^x	4.112 (5)	O23—O1	2.495 (5)
P—P^xi	4.250 (6)	O23—O1^xi	3.403 (7)
P—P^xii	4.222 (6)	O23—O1^xii	3.305 (7)
P—P^xiv	4.046 (4)	O1—PB1^viii	3.028 (7)
P—O21	1.558 (6)	O1—PB1^ix	3.523 (7)
P—O21^xv	4.499 (5)	O1—PB1^vi	3.105 (5)
P—O21^x	4.296 (6)	O1—PB2	2.365 (5)
P—O21^xi	4.297 (7)	O1—PB2^x	4.055 (6)
P—O21^xvi	4.392 (5)	O1—PB2^xi	4.343 (5)
P—O21^xiv	3.755 (6)	O1—PB2^xii	4.030 (6)
P—O22	1.545 (6)	O1—P	1.493 (4)
P—O22^x	4.027 (6)	O1—P^x	3.387 (6)
P—O22^xii	4.243 (7)	O1—P^xi	3.380 (7)
P—O22^xvii	4.204 (5)	O1—P^xii	3.537 (7)
P—O22^xiv	3.982 (6)	O1—O21	2.491 (6)
P—O23	1.566 (5)	O1—O21^x	3.298 (6)
P—O23^xi	4.446 (7)	O1—O21^xi	3.206 (7)
P—O23^xii	4.217 (7)	O1—O22	2.483 (6)
P—O23^xviii	4.477 (6)	O1—O22^x	3.131 (5)
P—O23^xix	4.250 (6)	O1—O22^xii	3.338 (7)
P—O23^xiv	3.728 (6)	O1—O23	2.495 (5)
P—O1	1.493 (4)	O1—O23^xi	3.403 (7)
P—O1^x	3.387 (6)	O1—O23^xii	3.305 (7)
P—O1^xi	3.380 (7)	O1—O1^x	3.230 (9)
P—O1^xii	3.537 (7)	O1—O1^xi	3.040 (10)
O21—PB1^viii	2.555 (5)	O1—O1^xii	3.413 (10)
O21—PB1^vi	4.418 (5)
O21—P—O22	109.51 (9)	O22—P—O23	109.43 (9)
O21—P—O23	109.58 (9)	O22—P—O1	109.56 (9)
O21—P—O1	109.44 (9)	O23—P—O1	109.32 (10)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, −y+1, z+3/2; (xviii) x, −y, z+1/2; (xix) x, −y+1, z+1/2; (xx) x, y−1, z; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2.

(S2P6_phase_1)

Crystal data

O8P2Pb3	V = 716.94 (9) Å^3
Mr = 811.74	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7854 (12) Å	T = 298 K
b = 5.6547 (6) Å	Particle morphology: plate
c = 9.4204 (9) Å	irregular, 6 × 6 mm
β = 102.497 (10)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), 2.92 < d <3.025 Angstrom (contamination from unidentified phase), d > 3.73 Angstrom (no useful data)
Rp = 0.063	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 96.1 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 4.12 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 146.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 287.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.051	50 parameters
Rexp = 0.054	10 restraints
R(F^2) = 0.17400	(Δ/σ)max = 0.01
χ^2 = 0.922	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.115500 2: -2.240590E-02 3: 7.059650E-02 4: -2.216800E-02 5: 2.758360E-02 6: -1.757150E-02 7: 1.267790E-02 8: -7.667760E-03 9: 9.145050E-0310: -3.381540E-0311: 1.423600E-0312: -2.984270E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89810 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
PB1	0.0	0.282 (2)	0.25	0.0185 (18)*
PB2	0.3168 (4)	0.3084 (14)	0.3489 (9)	0.0185 (18)*
P	0.6015 (3)	0.2532 (13)	0.4486 (6)	0.015 (3)*
O21	0.6461 (6)	0.0258 (18)	0.3964 (12)	0.0132 (16)*
O22	0.6311 (6)	0.4685 (18)	0.3677 (10)	0.0132 (16)*
O23	0.6416 (7)	0.2843 (18)	0.6135 (8)	0.0132 (16)*
O1	0.4887 (4)	0.2325 (18)	0.4172 (11)	0.0132 (16)*

Geometric parameters (Å, º)

PB1—PB2	4.266 (5)	O21—PB2^xi	3.010 (14)
PB1—PB2^i	4.266 (5)	O21—PB2^xii	4.434 (11)
PB1—PB2^ii	3.928 (12)	O21—PB2^viii	2.775 (10)
PB1—PB2^iii	4.140 (12)	O21—PB2^xiii	4.499 (13)
PB1—PB2^iv	3.928 (12)	O21—P^xix	4.454 (8)
PB1—PB2^v	4.140 (12)	O21—P	1.550 (8)
PB1—PB2^vi	4.097 (7)	O21—P^x	4.366 (14)
PB1—PB2^vii	4.097 (7)	O21—P^xi	4.293 (12)
PB1—P^ii	3.641 (12)	O21—P^xx	4.420 (9)
PB1—P^iii	3.381 (11)	O21—P^xiv	3.688 (12)
PB1—P^iv	3.641 (12)	O21—O21^x	4.362 (19)
PB1—P^v	3.381 (11)	O21—O21^xxi	4.40 (2)
PB1—P^vi	3.432 (5)	O21—O21^xiv	4.003 (19)
PB1—P^vii	3.432 (5)	O21—O22^xix	3.166 (9)
PB1—O21^iii	2.581 (11)	O21—O22	2.522 (9)
PB1—O21^v	2.581 (11)	O21—O22^xxii	4.363 (10)
PB1—O21^vi	4.386 (10)	O21—O22^xiv	3.379 (14)
PB1—O21^vii	4.386 (10)	O21—O23	2.525 (9)
PB1—O22^ii	2.601 (13)	O21—O23^xi	4.319 (12)
PB1—O22^iii	4.326 (15)	O21—O23^xx	3.179 (13)
PB1—O22^iv	2.601 (13)	O21—O23^xiv	3.138 (12)
PB1—O22^v	4.326 (15)	O21—O1	2.510 (8)
PB1—O23^vi	2.586 (10)	O21—O1^x	3.342 (12)
PB1—O23^vii	2.586 (10)	O21—O1^xi	3.175 (13)
PB1—O1^ii	3.501 (14)	O22—PB1^viii	4.326 (15)
PB1—O1^iii	3.018 (13)	O22—PB1^ix	2.601 (13)
PB1—O1^iv	3.501 (14)	O22—PB2	4.393 (10)
PB1—O1^v	3.018 (13)	O22—PB2^x	2.477 (13)
PB1—O1^vi	3.106 (10)	O22—PB2^xii	2.899 (13)
PB1—O1^vii	3.106 (10)	O22—PB2^ix	3.236 (9)
PB2—PB1	4.266 (5)	O22—P	1.538 (8)
PB2—PB1^viii	4.140 (12)	O22—P^x	4.063 (12)
PB2—PB1^ix	3.928 (12)	O22—P^xii	4.260 (13)
PB2—PB1^vi	4.097 (7)	O22—P^xviii	4.187 (8)
PB2—PB2^iv	3.657 (8)	O22—P^xiv	3.924 (12)
PB2—PB2^v	3.657 (8)	O22—O21	2.522 (9)
PB2—PB2^vi	3.768 (16)	O22—O21^xv	3.166 (9)
PB2—P	3.846 (7)	O22—O21^xxiii	4.363 (10)
PB2—P^x	3.254 (10)	O22—O21^xiv	3.379 (14)
PB2—P^xi	3.750 (10)	O22—O22^x	3.809 (17)
PB2—P^xii	3.182 (10)	O22—O22^xiv	4.420 (18)
PB2—P^iii	4.150 (10)	O22—O23	2.514 (9)
PB2—P^vii	4.278 (9)	O22—O23^xii	4.050 (14)
PB2—O21^x	2.944 (14)	O22—O23^xviii	2.804 (13)
PB2—O21^xi	3.010 (14)	O22—O23^xiv	3.414 (14)
PB2—O21^xii	4.434 (11)	O22—O1	2.500 (8)
PB2—O21^iii	2.775 (10)	O22—O1^x	3.130 (11)
PB2—O21^vii	4.499 (13)	O22—O1^xii	3.337 (15)
PB2—O22	4.393 (10)	O23—PB1^vi	2.586 (10)
PB2—O22^x	2.477 (13)	O23—PB2^xi	3.406 (12)
PB2—O22^xii	2.899 (13)	O23—PB2^xii	2.382 (12)
PB2—O22^ii	3.236 (9)	O23—PB2^xiii	2.951 (9)
PB2—O23^xi	3.406 (12)	O23—P	1.542 (8)
PB2—O23^xii	2.382 (12)	O23—P^xi	4.468 (13)
PB2—O23^vii	2.951 (9)	O23—P^xii	4.191 (14)
PB2—O1	2.357 (8)	O23—P^xvii	4.227 (12)
PB2—O1^x	4.071 (12)	O23—P^xiv	3.719 (12)
PB2—O1^xi	4.341 (12)	O23—O21	2.525 (9)
PB2—O1^xii	4.029 (12)	O23—O21^xi	4.319 (12)
P—PB1^viii	3.381 (11)	O23—O21^xvi	3.179 (13)
P—PB1^ix	3.641 (12)	O23—O21^xiv	3.138 (12)
P—PB1^vi	3.432 (5)	O23—O22	2.514 (9)
P—PB2	3.846 (7)	O23—O22^xii	4.050 (14)
P—PB2^x	3.254 (10)	O23—O22^xvii	2.804 (13)
P—PB2^xi	3.750 (10)	O23—O22^xiv	3.414 (14)
P—PB2^xii	3.182 (10)	O23—O23^xxiv	4.496 (12)
P—PB2^viii	4.150 (10)	O23—O23^xxv	4.496 (12)
P—PB2^xiii	4.278 (9)	O23—O23^xiv	4.05 (2)
P—P^x	4.159 (11)	O23—O1	2.502 (8)
P—P^xi	4.259 (11)	O23—O1^xi	3.409 (15)
P—P^xii	4.211 (12)	O23—O1^xii	3.248 (15)
P—P^xiv	3.999 (8)	O1—PB1^viii	3.018 (13)
P—O21	1.550 (8)	O1—PB1^ix	3.501 (14)
P—O21^xv	4.454 (8)	O1—PB1^vi	3.106 (10)
P—O21^x	4.366 (14)	O1—PB2	2.357 (8)
P—O21^xi	4.293 (12)	O1—PB2^x	4.071 (12)
P—O21^xvi	4.420 (9)	O1—PB2^xi	4.341 (12)
P—O21^xiv	3.688 (12)	O1—PB2^xii	4.029 (12)
P—O22	1.538 (8)	O1—P	1.523 (6)
P—O22^x	4.063 (12)	O1—P^x	3.403 (13)
P—O22^xii	4.260 (13)	O1—P^xi	3.371 (15)
P—O22^xvii	4.187 (8)	O1—P^xii	3.504 (15)
P—O22^xiv	3.924 (12)	O1—O21	2.510 (8)
P—O23	1.542 (8)	O1—O21^x	3.342 (12)
P—O23^xi	4.468 (13)	O1—O21^xi	3.175 (13)
P—O23^xii	4.191 (14)	O1—O22	2.500 (8)
P—O23^xviii	4.227 (12)	O1—O22^x	3.130 (11)
P—O23^xiv	3.719 (12)	O1—O22^xii	3.337 (15)
P—O1	1.523 (6)	O1—O23	2.502 (8)
P—O1^x	3.403 (13)	O1—O23^xi	3.409 (15)
P—O1^xi	3.371 (15)	O1—O23^xii	3.248 (15)
P—O1^xii	3.504 (15)	O1—O1^x	3.23 (2)
O21—PB1^viii	2.581 (11)	O1—O1^xi	3.04 (2)
O21—PB1^vi	4.386 (10)	O1—O1^xii	3.39 (2)
O21—PB2^x	2.944 (14)
O21—P—O22	109.47 (11)	O22—P—O23	109.45 (10)
O21—P—O23	109.50 (10)	O22—P—O1	109.50 (11)
O21—P—O1	109.46 (11)	O23—P—O1	109.44 (12)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, −y+1, z+3/2; (xviii) x, −y+1, z+1/2; (xix) x, y−1, z; (xx) x, −y, z+1/2; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2; (xxiv) −x+3/2, y−1/2, −z+3/2; (xxv) −x+3/2, y+1/2, −z+3/2.

(S2P6_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.9005 (8) Å	T = 298 K
c = 2.8290 (13) Å	Particle morphology: Pressure cell anvil material
V = 20.61 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), 2.92 < d <3.025 Angstrom (contamination from unidentified phase), d > 3.73 Angstrom (no useful data)
Rp = 0.063	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 96.1 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 4.12 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 146.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 287.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.051	50 parameters
Rexp = 0.054	10 restraints
R(F^2) = 0.17400	(Δ/σ)max = 0.01
χ^2 = 0.922	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.115500 2: -2.240590E-02 3: 7.059650E-02 4: -2.216800E-02 5: 2.758360E-02 6: -1.757150E-02 7: 1.267790E-02 8: -7.667760E-03 9: 9.145050E-0310: -3.381540E-0311: 1.423600E-0312: -2.984270E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89810 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.266 (5)	O21—PB2	3.010 (14)
PB1—PB2^i	4.266 (5)	O21—PB2	4.434 (11)
PB1—PB2	3.928 (12)	O21—PB2	2.775 (10)
PB1—PB2	4.140 (12)	O21—PB2	4.499 (13)
PB1—PB2	3.928 (12)	O21—P^iv	4.454 (8)
PB1—PB2	4.140 (12)	O21—P	1.550 (8)
PB1—PB2	4.097 (7)	O21—P^ii	4.366 (14)
PB1—PB2	4.097 (7)	O21—P	4.293 (12)
PB1—P	3.641 (12)	O21—P	4.420 (9)
PB1—P	3.381 (11)	O21—P	3.688 (12)
PB1—P	3.641 (12)	O21—O21^ii	4.362 (19)
PB1—P	3.381 (11)	O21—O21	4.40 (2)
PB1—P	3.432 (5)	O21—O21	4.003 (19)
PB1—P	3.432 (5)	O21—O22^iv	3.166 (9)
PB1—O21	2.581 (11)	O21—O22	2.522 (9)
PB1—O21	2.581 (11)	O21—O22	4.363 (10)
PB1—O21	4.386 (10)	O21—O22	3.379 (14)
PB1—O21	4.386 (10)	O21—O23	2.525 (9)
PB1—O22	2.601 (13)	O21—O23	4.319 (12)
PB1—O22	4.326 (15)	O21—O23	3.179 (13)
PB1—O22	2.601 (13)	O21—O23	3.138 (12)
PB1—O22	4.326 (15)	O21—O1	2.510 (8)
PB1—O23	2.586 (10)	O21—O1^ii	3.342 (12)
PB1—O23	2.586 (10)	O21—O1	3.175 (13)
PB1—O1	3.501 (14)	O22—PB1	4.326 (15)
PB1—O1	3.018 (13)	O22—PB1	2.601 (13)
PB1—O1	3.501 (14)	O22—PB2	4.393 (10)
PB1—O1	3.018 (13)	O22—PB2^ii	2.477 (13)
PB1—O1	3.106 (10)	O22—PB2	2.899 (13)
PB1—O1	3.106 (10)	O22—PB2	3.236 (9)
PB2—PB1	4.266 (5)	O22—P	1.538 (8)
PB2—PB1	4.140 (12)	O22—P^ii	4.063 (12)
PB2—PB1	3.928 (12)	O22—P	4.260 (13)
PB2—PB1	4.097 (7)	O22—P	4.187 (8)
PB2—PB2	3.657 (8)	O22—P	3.924 (12)
PB2—PB2	3.657 (8)	O22—O21	2.522 (9)
PB2—PB2	3.768 (16)	O22—O21^iii	3.166 (9)
PB2—P	3.846 (7)	O22—O21	4.363 (10)
PB2—P^ii	3.254 (10)	O22—O21	3.379 (14)
PB2—P	3.750 (10)	O22—O22^ii	3.809 (17)
PB2—P	3.182 (10)	O22—O22	4.420 (18)
PB2—P	4.150 (10)	O22—O23	2.514 (9)
PB2—P	4.278 (9)	O22—O23	4.050 (14)
PB2—O21^ii	2.944 (14)	O22—O23	2.804 (13)
PB2—O21	3.010 (14)	O22—O23	3.414 (14)
PB2—O21	4.434 (11)	O22—O1	2.500 (8)
PB2—O21	2.775 (10)	O22—O1^ii	3.130 (11)
PB2—O21	4.499 (13)	O22—O1	3.337 (15)
PB2—O22	4.393 (10)	O23—PB1	2.586 (10)
PB2—O22^ii	2.477 (13)	O23—PB2	3.406 (12)
PB2—O22	2.899 (13)	O23—PB2	2.382 (12)
PB2—O22	3.236 (9)	O23—PB2	2.951 (9)
PB2—O23	3.406 (12)	O23—P	1.542 (8)
PB2—O23	2.382 (12)	O23—P	4.468 (13)
PB2—O23	2.951 (9)	O23—P	4.191 (14)
PB2—O1	2.357 (8)	O23—P	4.227 (12)
PB2—O1^ii	4.071 (12)	O23—P	3.719 (12)
PB2—O1	4.341 (12)	O23—O21	2.525 (9)
PB2—O1	4.029 (12)	O23—O21	4.319 (12)
P—PB1	3.381 (11)	O23—O21	3.179 (13)
P—PB1	3.641 (12)	O23—O21	3.138 (12)
P—PB1	3.432 (5)	O23—O22	2.514 (9)
P—PB2	3.846 (7)	O23—O22	4.050 (14)
P—PB2^ii	3.254 (10)	O23—O22	2.804 (13)
P—PB2	3.750 (10)	O23—O22	3.414 (14)
P—PB2	3.182 (10)	O23—O23	4.496 (12)
P—PB2	4.150 (10)	O23—O23	4.496 (12)
P—PB2	4.278 (9)	O23—O23	4.05 (2)
P—P^ii	4.159 (11)	O23—O1	2.502 (8)
P—P	4.259 (11)	O23—O1	3.409 (15)
P—P	4.211 (12)	O23—O1	3.248 (15)
P—P	3.999 (8)	O1—PB1	3.018 (13)
P—O21	1.550 (8)	O1—PB1	3.501 (14)
P—O21^iii	4.454 (8)	O1—PB1	3.106 (10)
P—O21^ii	4.366 (14)	O1—PB2	2.357 (8)
P—O21	4.293 (12)	O1—PB2^ii	4.071 (12)
P—O21	4.420 (9)	O1—PB2	4.341 (12)
P—O21	3.688 (12)	O1—PB2	4.029 (12)
P—O22	1.538 (8)	O1—P	1.523 (6)
P—O22^ii	4.063 (12)	O1—P^ii	3.403 (13)
P—O22	4.260 (13)	O1—P	3.371 (15)
P—O22	4.187 (8)	O1—P	3.504 (15)
P—O22	3.924 (12)	O1—O21	2.510 (8)
P—O23	1.542 (8)	O1—O21^ii	3.342 (12)
P—O23	4.468 (13)	O1—O21	3.175 (13)
P—O23	4.191 (14)	O1—O22	2.500 (8)
P—O23	4.227 (12)	O1—O22^ii	3.130 (11)
P—O23	3.719 (12)	O1—O22	3.337 (15)
P—O1	1.523 (6)	O1—O23	2.502 (8)
P—O1^ii	3.403 (13)	O1—O23	3.409 (15)
P—O1	3.371 (15)	O1—O23	3.248 (15)
P—O1	3.504 (15)	O1—O1^ii	3.23 (2)
O21—PB1	2.581 (11)	O1—O1	3.04 (2)
O21—PB1	4.386 (10)	O1—O1	3.39 (2)
O21—PB2^ii	2.944 (14)
O21—P—O22	109.47 (11)	O22—P—O23	109.45 (10)
O21—P—O23	109.50 (10)	O22—P—O1	109.50 (11)
O21—P—O1	109.46 (11)	O23—P—O1	109.44 (12)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(S2P6_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5620 (8) Å	Particle morphology: Component of pressure cell, not sample
V = 45.20 (3) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), 2.92 < d <3.025 Angstrom (contamination from unidentified phase), d > 3.73 Angstrom (no useful data)
Rp = 0.063	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 96.1 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 4.12 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 146.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 287.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.051	50 parameters
Rexp = 0.054	10 restraints
R(F^2) = 0.17400	(Δ/σ)max = 0.01
χ^2 = 0.922	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.115500 2: -2.240590E-02 3: 7.059650E-02 4: -2.216800E-02 5: 2.758360E-02 6: -1.757150E-02 7: 1.267790E-02 8: -7.667760E-03 9: 9.145050E-0310: -3.381540E-0311: 1.423600E-0312: -2.984270E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89810 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.266 (5)	O21—PB2^xi	3.010 (14)
PB1—PB2^i	4.266 (5)	O21—PB2^xii	4.434 (11)
PB1—PB2^ii	3.928 (12)	O21—PB2^viii	2.775 (10)
PB1—PB2^iii	4.140 (12)	O21—PB2^xiii	4.499 (13)
PB1—PB2^iv	3.928 (12)	O21—P^xix	4.454 (8)
PB1—PB2^v	4.140 (12)	O21—P	1.550 (8)
PB1—PB2^vi	4.097 (7)	O21—P^x	4.366 (14)
PB1—PB2^vii	4.097 (7)	O21—P^xi	4.293 (12)
PB1—P^ii	3.641 (12)	O21—P^xx	4.420 (9)
PB1—P^iii	3.381 (11)	O21—P^xiv	3.688 (12)
PB1—P^iv	3.641 (12)	O21—O21^x	4.362 (19)
PB1—P^v	3.381 (11)	O21—O21^xxi	4.40 (2)
PB1—P^vi	3.432 (5)	O21—O21^xiv	4.003 (19)
PB1—P^vii	3.432 (5)	O21—O22^xix	3.166 (9)
PB1—O21^iii	2.581 (11)	O21—O22	2.522 (9)
PB1—O21^v	2.581 (11)	O21—O22^xxii	4.363 (10)
PB1—O21^vi	4.386 (10)	O21—O22^xiv	3.379 (14)
PB1—O21^vii	4.386 (10)	O21—O23	2.525 (9)
PB1—O22^ii	2.601 (13)	O21—O23^xi	4.319 (12)
PB1—O22^iii	4.326 (15)	O21—O23^xx	3.179 (13)
PB1—O22^iv	2.601 (13)	O21—O23^xiv	3.138 (12)
PB1—O22^v	4.326 (15)	O21—O1	2.510 (8)
PB1—O23^vi	2.586 (10)	O21—O1^x	3.342 (12)
PB1—O23^vii	2.586 (10)	O21—O1^xi	3.175 (13)
PB1—O1^ii	3.501 (14)	O22—PB1^viii	4.326 (15)
PB1—O1^iii	3.018 (13)	O22—PB1^ix	2.601 (13)
PB1—O1^iv	3.501 (14)	O22—PB2	4.393 (10)
PB1—O1^v	3.018 (13)	O22—PB2^x	2.477 (13)
PB1—O1^vi	3.106 (10)	O22—PB2^xii	2.899 (13)
PB1—O1^vii	3.106 (10)	O22—PB2^ix	3.236 (9)
PB2—PB1	4.266 (5)	O22—P	1.538 (8)
PB2—PB1^viii	4.140 (12)	O22—P^x	4.063 (12)
PB2—PB1^ix	3.928 (12)	O22—P^xii	4.260 (13)
PB2—PB1^vi	4.097 (7)	O22—P^xviii	4.187 (8)
PB2—PB2^iv	3.657 (8)	O22—P^xiv	3.924 (12)
PB2—PB2^v	3.657 (8)	O22—O21	2.522 (9)
PB2—PB2^vi	3.768 (16)	O22—O21^xv	3.166 (9)
PB2—P	3.846 (7)	O22—O21^xxiii	4.363 (10)
PB2—P^x	3.254 (10)	O22—O21^xiv	3.379 (14)
PB2—P^xi	3.750 (10)	O22—O22^x	3.809 (17)
PB2—P^xii	3.182 (10)	O22—O22^xiv	4.420 (18)
PB2—P^iii	4.150 (10)	O22—O23	2.514 (9)
PB2—P^vii	4.278 (9)	O22—O23^xii	4.050 (14)
PB2—O21^x	2.944 (14)	O22—O23^xviii	2.804 (13)
PB2—O21^xi	3.010 (14)	O22—O23^xiv	3.414 (14)
PB2—O21^xii	4.434 (11)	O22—O1	2.500 (8)
PB2—O21^iii	2.775 (10)	O22—O1^x	3.130 (11)
PB2—O21^vii	4.499 (13)	O22—O1^xii	3.337 (15)
PB2—O22	4.393 (10)	O23—PB1^vi	2.586 (10)
PB2—O22^x	2.477 (13)	O23—PB2^xi	3.406 (12)
PB2—O22^xii	2.899 (13)	O23—PB2^xii	2.382 (12)
PB2—O22^ii	3.236 (9)	O23—PB2^xiii	2.951 (9)
PB2—O23^xi	3.406 (12)	O23—P	1.542 (8)
PB2—O23^xii	2.382 (12)	O23—P^xi	4.468 (13)
PB2—O23^vii	2.951 (9)	O23—P^xii	4.191 (14)
PB2—O1	2.357 (8)	O23—P^xvii	4.227 (12)
PB2—O1^x	4.071 (12)	O23—P^xiv	3.719 (12)
PB2—O1^xi	4.341 (12)	O23—O21	2.525 (9)
PB2—O1^xii	4.029 (12)	O23—O21^xi	4.319 (12)
P—PB1^viii	3.381 (11)	O23—O21^xvi	3.179 (13)
P—PB1^ix	3.641 (12)	O23—O21^xiv	3.138 (12)
P—PB1^vi	3.432 (5)	O23—O22	2.514 (9)
P—PB2	3.846 (7)	O23—O22^xii	4.050 (14)
P—PB2^x	3.254 (10)	O23—O22^xvii	2.804 (13)
P—PB2^xi	3.750 (10)	O23—O22^xiv	3.414 (14)
P—PB2^xii	3.182 (10)	O23—O23^xxiv	4.496 (12)
P—PB2^viii	4.150 (10)	O23—O23^xxv	4.496 (12)
P—PB2^xiii	4.278 (9)	O23—O23^xiv	4.05 (2)
P—P^x	4.159 (11)	O23—O1	2.502 (8)
P—P^xi	4.259 (11)	O23—O1^xi	3.409 (15)
P—P^xii	4.211 (12)	O23—O1^xii	3.248 (15)
P—P^xiv	3.999 (8)	O1—PB1^viii	3.018 (13)
P—O21	1.550 (8)	O1—PB1^ix	3.501 (14)
P—O21^xv	4.454 (8)	O1—PB1^vi	3.106 (10)
P—O21^x	4.366 (14)	O1—PB2	2.357 (8)
P—O21^xi	4.293 (12)	O1—PB2^x	4.071 (12)
P—O21^xvi	4.420 (9)	O1—PB2^xi	4.341 (12)
P—O21^xiv	3.688 (12)	O1—PB2^xii	4.029 (12)
P—O22	1.538 (8)	O1—P	1.523 (6)
P—O22^x	4.063 (12)	O1—P^x	3.403 (13)
P—O22^xii	4.260 (13)	O1—P^xi	3.371 (15)
P—O22^xvii	4.187 (8)	O1—P^xii	3.504 (15)
P—O22^xiv	3.924 (12)	O1—O21	2.510 (8)
P—O23	1.542 (8)	O1—O21^x	3.342 (12)
P—O23^xi	4.468 (13)	O1—O21^xi	3.175 (13)
P—O23^xii	4.191 (14)	O1—O22	2.500 (8)
P—O23^xviii	4.227 (12)	O1—O22^x	3.130 (11)
P—O23^xiv	3.719 (12)	O1—O22^xii	3.337 (15)
P—O1	1.523 (6)	O1—O23	2.502 (8)
P—O1^x	3.403 (13)	O1—O23^xi	3.409 (15)
P—O1^xi	3.371 (15)	O1—O23^xii	3.248 (15)
P—O1^xii	3.504 (15)	O1—O1^x	3.23 (2)
O21—PB1^viii	2.581 (11)	O1—O1^xi	3.04 (2)
O21—PB1^vi	4.386 (10)	O1—O1^xii	3.39 (2)
O21—PB2^x	2.944 (14)
O21—P—O22	109.47 (11)	O22—P—O23	109.45 (10)
O21—P—O23	109.50 (10)	O22—P—O1	109.50 (11)
O21—P—O1	109.46 (11)	O23—P—O1	109.44 (12)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) x, y+1, z; (xvi) −z, −x, −y+1; (xvii) −z, −x+1, −y+1; (xviii) −z, −x+1, −y; (xix) x, y−1, z; (xx) −z, −x, −y; (xxi) −x+1, −y−1/2, −z+3/2; (xxii) z+1, x−1/2, y+1/2; (xxiii) z+1, x+1/2, y+1/2; (xxiv) z+1, x−1/2, y+3/2; (xxv) z+1, x+1/2, y+3/2.

(S2P12_phase_1)

Crystal data

O8P2Pb3	V = 702.22 (7) Å^3
Mr = 811.74	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7590 (9) Å	T = 298 K
b = 5.5526 (5) Å	Particle morphology: plate
c = 9.4305 (6) Å	irregular, 6 × 6 mm
β = 102.923 (9)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), 2.92 < d <3.025 Angstrom (contamination from unidentified phase), d > 3.73 Angstrom (no useful data)
Rp = 0.043	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 106.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.87 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 142.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 191.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.038	50 parameters
Rexp = 0.041	10 restraints
R(F^2) = 0.16761	(Δ/σ)max = 0.10
χ^2 = 0.922	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.413293 2: -0.114106 3: 0.243614 4: -0.102176 5: 9.262000E-02 6: -8.879140E-02 7: 4.811060E-02 8: -5.129760E-02 9: 4.228950E-0210: -3.231980E-0211: 1.082110E-0212: -7.293950E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89815 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
PB1	0.0	0.268 (2)	0.25	0.0209 (13)*
PB2	0.3159 (3)	0.2990 (12)	0.3502 (9)	0.0209 (13)*
P	0.6032 (2)	0.2595 (12)	0.4519 (5)	0.0109 (15)*
O21	0.6450 (6)	0.0231 (17)	0.3986 (9)	0.0154 (10)*
O22	0.6389 (6)	0.4746 (18)	0.3781 (10)	0.0154 (10)*
O23	0.6402 (6)	0.2820 (15)	0.6166 (8)	0.0154 (10)*
O1	0.4901 (3)	0.2520 (18)	0.4139 (10)	0.0154 (10)*

Geometric parameters (Å, º)

PB1—PB2	4.240 (4)	O21—PB1^vi	4.389 (9)
PB1—PB2^i	4.240 (4)	O21—PB2^x	2.950 (13)
PB1—PB2^ii	3.895 (10)	O21—PB2^xi	2.921 (12)
PB1—PB2^iii	4.131 (11)	O21—PB2^xii	4.416 (10)
PB1—PB2^iv	3.895 (10)	O21—PB2^viii	2.787 (9)
PB1—PB2^v	4.131 (11)	O21—PB2^xiii	4.491 (11)
PB1—PB2^vi	4.062 (7)	O21—P^xvii	4.323 (7)
PB1—PB2^vii	4.062 (7)	O21—P	1.561 (7)
PB1—P^ii	3.523 (10)	O21—P^x	4.388 (10)
PB1—P^iii	3.445 (10)	O21—P^xi	4.273 (11)
PB1—P^iv	3.523 (10)	O21—P^xix	4.411 (7)
PB1—P^v	3.445 (10)	O21—P^xiv	3.643 (11)
PB1—P^vi	3.424 (5)	O21—O21^x	4.332 (17)
PB1—P^vii	3.424 (5)	O21—O21^xxi	4.329 (18)
PB1—O21^iii	2.587 (11)	O21—O21^xiv	3.986 (18)
PB1—O21^v	2.587 (11)	O21—O22^xvii	3.052 (8)
PB1—O21^vi	4.389 (9)	O21—O22	2.514 (8)
PB1—O21^vii	4.389 (9)	O21—O22^xxii	4.381 (8)
PB1—O22^ii	2.596 (12)	O21—O22^xiv	3.237 (12)
PB1—O22^iii	4.412 (13)	O21—O23	2.522 (7)
PB1—O22^iv	2.596 (12)	O21—O23^xi	4.247 (12)
PB1—O22^v	4.412 (13)	O21—O23^xix	3.141 (11)
PB1—O23^ii	4.470 (10)	O21—O23^xiv	3.181 (12)
PB1—O23^iv	4.470 (10)	O21—O1	2.513 (7)
PB1—O23^vi	2.543 (9)	O21—O1^x	3.362 (10)
PB1—O23^vii	2.543 (9)	O21—O1^xi	3.223 (12)
PB1—O1^ii	3.274 (13)	O22—PB1^viii	4.412 (13)
PB1—O1^iii	3.117 (13)	O22—PB1^ix	2.596 (12)
PB1—O1^iv	3.274 (13)	O22—PB2	4.500 (9)
PB1—O1^v	3.117 (13)	O22—PB2^x	2.564 (13)
PB1—O1^vi	3.144 (10)	O22—PB2^xii	2.796 (13)
PB1—O1^vii	3.144 (10)	O22—PB2^ix	3.087 (8)
PB2—PB1	4.240 (4)	O22—P	1.519 (8)
PB2—PB1^viii	4.131 (11)	O22—P^xv	4.458 (8)
PB2—PB1^ix	3.895 (10)	O22—P^x	4.191 (11)
PB2—PB1^vi	4.062 (7)	O22—P^xii	4.270 (13)
PB2—PB2^iv	3.610 (7)	O22—P^xx	4.206 (7)
PB2—PB2^v	3.610 (7)	O22—P^xiv	3.783 (11)
PB2—PB2^vi	3.723 (15)	O22—O21	2.514 (8)
PB2—P	3.859 (5)	O22—O21^xv	3.052 (8)
PB2—P^x	3.290 (10)	O22—O21^xxiii	4.381 (8)
PB2—P^xi	3.662 (8)	O22—O21^xiv	3.237 (12)
PB2—P^xii	3.131 (9)	O22—O22^x	4.040 (17)
PB2—P^ii	4.440 (8)	O22—O22^xiv	4.208 (18)
PB2—P^iii	4.157 (8)	O22—O23	2.487 (8)
PB2—P^vii	4.227 (7)	O22—O23^xii	4.081 (12)
PB2—O21^x	2.950 (13)	O22—O23^xx	2.815 (10)
PB2—O21^xi	2.921 (12)	O22—O23^xiv	3.347 (12)
PB2—O21^xii	4.416 (10)	O22—O1	2.478 (8)
PB2—O21^iii	2.787 (9)	O22—O1^x	3.174 (10)
PB2—O21^vii	4.491 (11)	O22—O1^xii	3.296 (15)
PB2—O22	4.500 (9)	O23—PB1^ix	4.470 (10)
PB2—O22^x	2.564 (13)	O23—PB1^vi	2.543 (9)
PB2—O22^xii	2.796 (13)	O23—PB2^xi	3.284 (9)
PB2—O22^ii	3.087 (8)	O23—PB2^xii	2.406 (9)
PB2—O23^xi	3.284 (9)	O23—PB2^xiii	2.919 (8)
PB2—O23^xii	2.406 (9)	O23—P	1.528 (7)
PB2—O23^vii	2.919 (8)	O23—P^xi	4.438 (12)
PB2—O1	2.352 (6)	O23—P^xii	4.140 (11)
PB2—O1^x	4.046 (11)	O23—P^xvi	4.474 (11)
PB2—O1^xi	4.333 (11)	O23—P^xviii	4.178 (10)
PB2—O1^xii	3.954 (11)	O23—P^xiv	3.737 (10)
P—PB1^viii	3.445 (10)	O23—O21	2.522 (7)
P—PB1^ix	3.523 (10)	O23—O21^xi	4.247 (12)
P—PB1^vi	3.424 (5)	O23—O21^xvi	3.141 (11)
P—PB2	3.859 (5)	O23—O21^xiv	3.181 (12)
P—PB2^x	3.290 (10)	O23—O22	2.487 (8)
P—PB2^xi	3.662 (8)	O23—O22^xii	4.081 (12)
P—PB2^xii	3.131 (9)	O23—O22^xviii	2.815 (10)
P—PB2^viii	4.157 (8)	O23—O22^xiv	3.347 (12)
P—PB2^ix	4.440 (8)	O23—O23^xxiv	4.446 (11)
P—PB2^xiii	4.227 (7)	O23—O23^xxv	4.446 (11)
P—P^x	4.210 (8)	O23—O23^xiv	4.132 (18)
P—P^xi	4.282 (10)	O23—O1	2.486 (7)
P—P^xii	4.143 (11)	O23—O1^xi	3.444 (14)
P—P^xiv	3.940 (6)	O23—O1^xii	3.124 (13)
P—O21	1.561 (7)	O1—PB1^viii	3.117 (13)
P—O21^xv	4.323 (7)	O1—PB1^ix	3.274 (13)
P—O21^x	4.388 (10)	O1—PB1^vi	3.144 (10)
P—O21^xi	4.273 (11)	O1—PB2	2.352 (6)
P—O21^xvi	4.411 (7)	O1—PB2^x	4.046 (11)
P—O21^xiv	3.643 (11)	O1—PB2^xi	4.333 (11)
P—O22^xvii	4.458 (8)	O1—PB2^xii	3.954 (11)
P—O22	1.519 (8)	O1—P	1.516 (5)
P—O22^x	4.191 (11)	O1—P^x	3.401 (12)
P—O22^xii	4.270 (13)	O1—P^xi	3.470 (13)
P—O22^xviii	4.206 (7)	O1—P^xii	3.366 (14)
P—O22^xiv	3.783 (11)	O1—O21	2.513 (7)
P—O23	1.528 (7)	O1—O21^x	3.362 (10)
P—O23^xi	4.438 (12)	O1—O21^xi	3.223 (12)
P—O23^xii	4.140 (11)	O1—O22	2.478 (8)
P—O23^xix	4.474 (11)	O1—O22^x	3.174 (10)
P—O23^xx	4.178 (10)	O1—O22^xii	3.296 (15)
P—O23^xiv	3.737 (10)	O1—O23	2.486 (7)
P—O1	1.516 (5)	O1—O23^xi	3.444 (14)
P—O1^x	3.401 (12)	O1—O23^xii	3.124 (13)
P—O1^xi	3.470 (13)	O1—O1^x	3.163 (19)
P—O1^xii	3.366 (14)	O1—O1^xi	3.217 (19)
O21—PB1^viii	2.587 (11)	O1—O1^xii	3.18 (2)
O21—P—O22	109.47 (11)	O22—P—O23	109.44 (10)
O21—P—O23	109.47 (10)	O22—P—O1	109.48 (11)
O21—P—O1	109.48 (11)	O23—P—O1	109.49 (11)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, y−1, z; (xviii) x, −y+1, z+3/2; (xix) x, −y, z+1/2; (xx) x, −y+1, z+1/2; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2; (xxiv) −x+3/2, y−1/2, −z+3/2; (xxv) −x+3/2, y+1/2, −z+3/2.

(S2P12_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8995 (6) Å	T = 298 K
c = 2.8302 (10) Å	Particle morphology: Pressure cell anvil material
V = 20.61 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), 2.92 < d <3.025 Angstrom (contamination from unidentified phase), d > 3.73 Angstrom (no useful data)
Rp = 0.043	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 106.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.87 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 142.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 191.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.038	50 parameters
Rexp = 0.041	10 restraints
R(F^2) = 0.16761	(Δ/σ)max = 0.10
χ^2 = 0.922	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.413293 2: -0.114106 3: 0.243614 4: -0.102176 5: 9.262000E-02 6: -8.879140E-02 7: 4.811060E-02 8: -5.129760E-02 9: 4.228950E-0210: -3.231980E-0211: 1.082110E-0212: -7.293950E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89815 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.240 (4)	O21—PB1	4.389 (9)
PB1—PB2^i	4.240 (4)	O21—PB2^ii	2.950 (13)
PB1—PB2	3.895 (10)	O21—PB2	2.921 (12)
PB1—PB2	4.131 (11)	O21—PB2	4.416 (10)
PB1—PB2	3.895 (10)	O21—PB2	2.787 (9)
PB1—PB2	4.131 (11)	O21—PB2	4.491 (11)
PB1—PB2	4.062 (7)	O21—P^iv	4.323 (7)
PB1—PB2	4.062 (7)	O21—P	1.561 (7)
PB1—P	3.523 (10)	O21—P^ii	4.388 (10)
PB1—P	3.445 (10)	O21—P	4.273 (11)
PB1—P	3.523 (10)	O21—P	4.411 (7)
PB1—P	3.445 (10)	O21—P	3.643 (11)
PB1—P	3.424 (5)	O21—O21^ii	4.332 (17)
PB1—P	3.424 (5)	O21—O21	4.329 (18)
PB1—O21	2.587 (11)	O21—O21	3.986 (18)
PB1—O21	2.587 (11)	O21—O22^iv	3.052 (8)
PB1—O21	4.389 (9)	O21—O22	2.514 (8)
PB1—O21	4.389 (9)	O21—O22	4.381 (8)
PB1—O22	2.596 (12)	O21—O22	3.237 (12)
PB1—O22	4.412 (13)	O21—O23	2.522 (7)
PB1—O22	2.596 (12)	O21—O23	4.247 (12)
PB1—O22	4.412 (13)	O21—O23	3.141 (11)
PB1—O23	4.470 (10)	O21—O23	3.181 (12)
PB1—O23	4.470 (10)	O21—O1	2.513 (7)
PB1—O23	2.543 (9)	O21—O1^ii	3.362 (10)
PB1—O23	2.543 (9)	O21—O1	3.223 (12)
PB1—O1	3.274 (13)	O22—PB1	4.412 (13)
PB1—O1	3.117 (13)	O22—PB1	2.596 (12)
PB1—O1	3.274 (13)	O22—PB2	4.500 (9)
PB1—O1	3.117 (13)	O22—PB2^ii	2.564 (13)
PB1—O1	3.144 (10)	O22—PB2	2.796 (13)
PB1—O1	3.144 (10)	O22—PB2	3.087 (8)
PB2—PB1	4.240 (4)	O22—P	1.519 (8)
PB2—PB1	4.131 (11)	O22—P^iii	4.458 (8)
PB2—PB1	3.895 (10)	O22—P^ii	4.191 (11)
PB2—PB1	4.062 (7)	O22—P	4.270 (13)
PB2—PB2	3.610 (7)	O22—P	4.206 (7)
PB2—PB2	3.610 (7)	O22—P	3.783 (11)
PB2—PB2	3.723 (15)	O22—O21	2.514 (8)
PB2—P	3.859 (5)	O22—O21^iii	3.052 (8)
PB2—P^ii	3.290 (10)	O22—O21	4.381 (8)
PB2—P	3.662 (8)	O22—O21	3.237 (12)
PB2—P	3.131 (9)	O22—O22^ii	4.040 (17)
PB2—P	4.440 (8)	O22—O22	4.208 (18)
PB2—P	4.157 (8)	O22—O23	2.487 (8)
PB2—P	4.227 (7)	O22—O23	4.081 (12)
PB2—O21^ii	2.950 (13)	O22—O23	2.815 (10)
PB2—O21	2.921 (12)	O22—O23	3.347 (12)
PB2—O21	4.416 (10)	O22—O1	2.478 (8)
PB2—O21	2.787 (9)	O22—O1^ii	3.174 (10)
PB2—O21	4.491 (11)	O22—O1	3.296 (15)
PB2—O22	4.500 (9)	O23—PB1	4.470 (10)
PB2—O22^ii	2.564 (13)	O23—PB1	2.543 (9)
PB2—O22	2.796 (13)	O23—PB2	3.284 (9)
PB2—O22	3.087 (8)	O23—PB2	2.406 (9)
PB2—O23	3.284 (9)	O23—PB2	2.919 (8)
PB2—O23	2.406 (9)	O23—P	1.528 (7)
PB2—O23	2.919 (8)	O23—P	4.438 (12)
PB2—O1	2.352 (6)	O23—P	4.140 (11)
PB2—O1^ii	4.046 (11)	O23—P	4.474 (11)
PB2—O1	4.333 (11)	O23—P	4.178 (10)
PB2—O1	3.954 (11)	O23—P	3.737 (10)
P—PB1	3.445 (10)	O23—O21	2.522 (7)
P—PB1	3.523 (10)	O23—O21	4.247 (12)
P—PB1	3.424 (5)	O23—O21	3.141 (11)
P—PB2	3.859 (5)	O23—O21	3.181 (12)
P—PB2^ii	3.290 (10)	O23—O22	2.487 (8)
P—PB2	3.662 (8)	O23—O22	4.081 (12)
P—PB2	3.131 (9)	O23—O22	2.815 (10)
P—PB2	4.157 (8)	O23—O22	3.347 (12)
P—PB2	4.440 (8)	O23—O23	4.446 (11)
P—PB2	4.227 (7)	O23—O23	4.446 (11)
P—P^ii	4.210 (8)	O23—O23	4.132 (18)
P—P	4.282 (10)	O23—O1	2.486 (7)
P—P	4.143 (11)	O23—O1	3.444 (14)
P—P	3.940 (6)	O23—O1	3.124 (13)
P—O21	1.561 (7)	O1—PB1	3.117 (13)
P—O21^iii	4.323 (7)	O1—PB1	3.274 (13)
P—O21^ii	4.388 (10)	O1—PB1	3.144 (10)
P—O21	4.273 (11)	O1—PB2	2.352 (6)
P—O21	4.411 (7)	O1—PB2^ii	4.046 (11)
P—O21	3.643 (11)	O1—PB2	4.333 (11)
P—O22^iv	4.458 (8)	O1—PB2	3.954 (11)
P—O22	1.519 (8)	O1—P	1.516 (5)
P—O22^ii	4.191 (11)	O1—P^ii	3.401 (12)
P—O22	4.270 (13)	O1—P	3.470 (13)
P—O22	4.206 (7)	O1—P	3.366 (14)
P—O22	3.783 (11)	O1—O21	2.513 (7)
P—O23	1.528 (7)	O1—O21^ii	3.362 (10)
P—O23	4.438 (12)	O1—O21	3.223 (12)
P—O23	4.140 (11)	O1—O22	2.478 (8)
P—O23	4.474 (11)	O1—O22^ii	3.174 (10)
P—O23	4.178 (10)	O1—O22	3.296 (15)
P—O23	3.737 (10)	O1—O23	2.486 (7)
P—O1	1.516 (5)	O1—O23	3.444 (14)
P—O1^ii	3.401 (12)	O1—O23	3.124 (13)
P—O1	3.470 (13)	O1—O1^ii	3.163 (19)
P—O1	3.366 (14)	O1—O1	3.217 (19)
O21—PB1	2.587 (11)	O1—O1	3.18 (2)
O21—P—O22	109.47 (11)	O22—P—O23	109.44 (10)
O21—P—O23	109.47 (10)	O22—P—O1	109.48 (11)
O21—P—O1	109.48 (11)	O23—P—O1	109.49 (11)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(S2P12_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5587 (5) Å	Particle morphology: Component of pressure cell, not sample
V = 45.07 (2) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), 2.92 < d <3.025 Angstrom (contamination from unidentified phase), d > 3.73 Angstrom (no useful data)
Rp = 0.043	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 106.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.87 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 142.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 191.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.038	50 parameters
Rexp = 0.041	10 restraints
R(F^2) = 0.16761	(Δ/σ)max = 0.10
χ^2 = 0.922	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.413293 2: -0.114106 3: 0.243614 4: -0.102176 5: 9.262000E-02 6: -8.879140E-02 7: 4.811060E-02 8: -5.129760E-02 9: 4.228950E-0210: -3.231980E-0211: 1.082110E-0212: -7.293950E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89815 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.240 (4)	O21—PB1^vi	4.389 (9)
PB1—PB2^i	4.240 (4)	O21—PB2^x	2.950 (13)
PB1—PB2^ii	3.895 (10)	O21—PB2^xi	2.921 (12)
PB1—PB2^iii	4.131 (11)	O21—PB2^xii	4.416 (10)
PB1—PB2^iv	3.895 (10)	O21—PB2^viii	2.787 (9)
PB1—PB2^v	4.131 (11)	O21—PB2^xiii	4.491 (11)
PB1—PB2^vi	4.062 (7)	O21—P^xvii	4.323 (7)
PB1—PB2^vii	4.062 (7)	O21—P	1.561 (7)
PB1—P^ii	3.523 (10)	O21—P^x	4.388 (10)
PB1—P^iii	3.445 (10)	O21—P^xi	4.273 (11)
PB1—P^iv	3.523 (10)	O21—P^xix	4.411 (7)
PB1—P^v	3.445 (10)	O21—P^xiv	3.643 (11)
PB1—P^vi	3.424 (5)	O21—O21^x	4.332 (17)
PB1—P^vii	3.424 (5)	O21—O21^xxi	4.329 (18)
PB1—O21^iii	2.587 (11)	O21—O21^xiv	3.986 (18)
PB1—O21^v	2.587 (11)	O21—O22^xvii	3.052 (8)
PB1—O21^vi	4.389 (9)	O21—O22	2.514 (8)
PB1—O21^vii	4.389 (9)	O21—O22^xxii	4.381 (8)
PB1—O22^ii	2.596 (12)	O21—O22^xiv	3.237 (12)
PB1—O22^iii	4.412 (13)	O21—O23	2.522 (7)
PB1—O22^iv	2.596 (12)	O21—O23^xi	4.247 (12)
PB1—O22^v	4.412 (13)	O21—O23^xix	3.141 (11)
PB1—O23^ii	4.470 (10)	O21—O23^xiv	3.181 (12)
PB1—O23^iv	4.470 (10)	O21—O1	2.513 (7)
PB1—O23^vi	2.543 (9)	O21—O1^x	3.362 (10)
PB1—O23^vii	2.543 (9)	O21—O1^xi	3.223 (12)
PB1—O1^ii	3.274 (13)	O22—PB1^viii	4.412 (13)
PB1—O1^iii	3.117 (13)	O22—PB1^ix	2.596 (12)
PB1—O1^iv	3.274 (13)	O22—PB2	4.500 (9)
PB1—O1^v	3.117 (13)	O22—PB2^x	2.564 (13)
PB1—O1^vi	3.144 (10)	O22—PB2^xii	2.796 (13)
PB1—O1^vii	3.144 (10)	O22—PB2^ix	3.087 (8)
PB2—PB1	4.240 (4)	O22—P	1.519 (8)
PB2—PB1^viii	4.131 (11)	O22—P^xv	4.458 (8)
PB2—PB1^ix	3.895 (10)	O22—P^x	4.191 (11)
PB2—PB1^vi	4.062 (7)	O22—P^xii	4.270 (13)
PB2—PB2^iv	3.610 (7)	O22—P^xx	4.206 (7)
PB2—PB2^v	3.610 (7)	O22—P^xiv	3.783 (11)
PB2—PB2^vi	3.723 (15)	O22—O21	2.514 (8)
PB2—P	3.859 (5)	O22—O21^xv	3.052 (8)
PB2—P^x	3.290 (10)	O22—O21^xxiii	4.381 (8)
PB2—P^xi	3.662 (8)	O22—O21^xiv	3.237 (12)
PB2—P^xii	3.131 (9)	O22—O22^x	4.040 (17)
PB2—P^ii	4.440 (8)	O22—O22^xiv	4.208 (18)
PB2—P^iii	4.157 (8)	O22—O23	2.487 (8)
PB2—P^vii	4.227 (7)	O22—O23^xii	4.081 (12)
PB2—O21^x	2.950 (13)	O22—O23^xx	2.815 (10)
PB2—O21^xi	2.921 (12)	O22—O23^xiv	3.347 (12)
PB2—O21^xii	4.416 (10)	O22—O1	2.478 (8)
PB2—O21^iii	2.787 (9)	O22—O1^x	3.174 (10)
PB2—O21^vii	4.491 (11)	O22—O1^xii	3.296 (15)
PB2—O22	4.500 (9)	O23—PB1^ix	4.470 (10)
PB2—O22^x	2.564 (13)	O23—PB1^vi	2.543 (9)
PB2—O22^xii	2.796 (13)	O23—PB2^xi	3.284 (9)
PB2—O22^ii	3.087 (8)	O23—PB2^xii	2.406 (9)
PB2—O23^xi	3.284 (9)	O23—PB2^xiii	2.919 (8)
PB2—O23^xii	2.406 (9)	O23—P	1.528 (7)
PB2—O23^vii	2.919 (8)	O23—P^xi	4.438 (12)
PB2—O1	2.352 (6)	O23—P^xii	4.140 (11)
PB2—O1^x	4.046 (11)	O23—P^xvi	4.474 (11)
PB2—O1^xi	4.333 (11)	O23—P^xviii	4.178 (10)
PB2—O1^xii	3.954 (11)	O23—P^xiv	3.737 (10)
P—PB1^viii	3.445 (10)	O23—O21	2.522 (7)
P—PB1^ix	3.523 (10)	O23—O21^xi	4.247 (12)
P—PB1^vi	3.424 (5)	O23—O21^xvi	3.141 (11)
P—PB2	3.859 (5)	O23—O21^xiv	3.181 (12)
P—PB2^x	3.290 (10)	O23—O22	2.487 (8)
P—PB2^xi	3.662 (8)	O23—O22^xii	4.081 (12)
P—PB2^xii	3.131 (9)	O23—O22^xviii	2.815 (10)
P—PB2^viii	4.157 (8)	O23—O22^xiv	3.347 (12)
P—PB2^ix	4.440 (8)	O23—O23^xxiv	4.446 (11)
P—PB2^xiii	4.227 (7)	O23—O23^xxv	4.446 (11)
P—P^x	4.210 (8)	O23—O23^xiv	4.132 (18)
P—P^xi	4.282 (10)	O23—O1	2.486 (7)
P—P^xii	4.143 (11)	O23—O1^xi	3.444 (14)
P—P^xiv	3.940 (6)	O23—O1^xii	3.124 (13)
P—O21	1.561 (7)	O1—PB1^viii	3.117 (13)
P—O21^xv	4.323 (7)	O1—PB1^ix	3.274 (13)
P—O21^x	4.388 (10)	O1—PB1^vi	3.144 (10)
P—O21^xi	4.273 (11)	O1—PB2	2.352 (6)
P—O21^xvi	4.411 (7)	O1—PB2^x	4.046 (11)
P—O21^xiv	3.643 (11)	O1—PB2^xi	4.333 (11)
P—O22^xvii	4.458 (8)	O1—PB2^xii	3.954 (11)
P—O22	1.519 (8)	O1—P	1.516 (5)
P—O22^x	4.191 (11)	O1—P^x	3.401 (12)
P—O22^xii	4.270 (13)	O1—P^xi	3.470 (13)
P—O22^xviii	4.206 (7)	O1—P^xii	3.366 (14)
P—O22^xiv	3.783 (11)	O1—O21	2.513 (7)
P—O23	1.528 (7)	O1—O21^x	3.362 (10)
P—O23^xi	4.438 (12)	O1—O21^xi	3.223 (12)
P—O23^xii	4.140 (11)	O1—O22	2.478 (8)
P—O23^xix	4.474 (11)	O1—O22^x	3.174 (10)
P—O23^xx	4.178 (10)	O1—O22^xii	3.296 (15)
P—O23^xiv	3.737 (10)	O1—O23	2.486 (7)
P—O1	1.516 (5)	O1—O23^xi	3.444 (14)
P—O1^x	3.401 (12)	O1—O23^xii	3.124 (13)
P—O1^xi	3.470 (13)	O1—O1^x	3.163 (19)
P—O1^xii	3.366 (14)	O1—O1^xi	3.217 (19)
O21—PB1^viii	2.587 (11)	O1—O1^xii	3.18 (2)
O21—P—O22	109.47 (11)	O22—P—O23	109.44 (10)
O21—P—O23	109.47 (10)	O22—P—O1	109.48 (11)
O21—P—O1	109.48 (11)	O23—P—O1	109.49 (11)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) x, y+1, z; (xvi) −z, −x, −y+1; (xvii) x, y−1, z; (xviii) −z, −x+1, −y+1; (xix) −z, −x, −y; (xx) −z, −x+1, −y; (xxi) −x+1, −y−1/2, −z+3/2; (xxii) z+1, x−1/2, y+1/2; (xxiii) z+1, x+1/2, y+1/2; (xxiv) z+1, x−1/2, y+3/2; (xxv) z+1, x+1/2, y+3/2.

(S2P14_phase_1)

Crystal data

O8P2Pb3	V = 698.08 (12) Å^3
Mr = 811.74	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7496 (14) Å	T = 298 K
b = 5.5234 (8) Å	Particle morphology: plate
c = 9.4344 (11) Å	irregular, 6 × 6 mm
β = 103.019 (14)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.586 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.63 Angstrom (no useful data)
Rp = 0.077	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 86.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 121.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 281.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.061	50 parameters
Rexp = 0.062	10 restraints
R(F^2) = 0.16735	(Δ/σ)max < 0.001
χ^2 = 0.980	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.121031 2: -4.985370E-02 3: 8.278980E-02 4: -4.438680E-02 5: 3.960540E-02 6: -3.841700E-02 7: 2.405080E-02 8: -2.353800E-02 9: 1.616540E-0210: -1.192490E-0211: 3.316930E-0312: -2.329230E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89802 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
PB1	0.0	0.257 (3)	0.25	0.022 (2)*
PB2	0.3159 (4)	0.2982 (19)	0.3458 (14)	0.022 (2)*
P	0.6035 (3)	0.2620 (17)	0.4511 (9)	0.015 (2)*
O21	0.6413 (10)	0.024 (3)	0.3971 (16)	0.0166 (17)*
O22	0.6440 (9)	0.476 (3)	0.3801 (15)	0.0166 (17)*
O23	0.6396 (10)	0.279 (2)	0.6161 (11)	0.0166 (17)*
O1	0.4906 (4)	0.266 (3)	0.4109 (18)	0.0166 (17)*

Geometric parameters (Å, º)

PB1—PB2	4.239 (5)	O21—PB2^x	2.92 (2)
PB1—PB2^i	4.239 (5)	O21—PB2^xi	2.96 (2)
PB1—PB2^ii	3.829 (16)	O21—PB2^xii	4.429 (16)
PB1—PB2^iii	4.148 (18)	O21—PB2^viii	2.841 (15)
PB1—PB2^iv	3.829 (16)	O21—PB2^xiii	4.481 (18)
PB1—PB2^v	4.148 (18)	O21—P^xvii	4.283 (11)
PB1—PB2^vi	4.085 (11)	O21—P	1.544 (9)
PB1—PB2^vii	4.085 (11)	O21—P^x	4.344 (17)
PB1—P^ii	3.445 (15)	O21—P^xi	4.25 (2)
PB1—P^iii	3.493 (16)	O21—P^xix	4.413 (12)
PB1—P^iv	3.445 (15)	O21—P^xiv	3.674 (17)
PB1—P^v	3.493 (16)	O21—O21^x	4.24 (3)
PB1—P^vi	3.435 (8)	O21—O21^xxi	4.39 (3)
PB1—P^vii	3.435 (8)	O21—O21^xiv	4.04 (3)
PB1—O21^iii	2.581 (18)	O21—O22^xvii	3.030 (10)
PB1—O21^v	2.581 (18)	O21—O22	2.505 (10)
PB1—O21^vi	4.387 (14)	O21—O22^xxii	4.371 (14)
PB1—O21^vii	4.387 (14)	O21—O22^xiv	3.215 (19)
PB1—O22^ii	2.595 (18)	O21—O23	2.507 (9)
PB1—O22^iii	4.49 (2)	O21—O23^xi	4.185 (19)
PB1—O22^iv	2.595 (18)	O21—O23^xix	3.130 (17)
PB1—O22^v	4.49 (2)	O21—O23^xiv	3.232 (19)
PB1—O23^ii	4.425 (16)	O21—O1	2.496 (9)
PB1—O23^iv	4.425 (16)	O21—O1^x	3.340 (16)
PB1—O23^vi	2.532 (15)	O21—O1^xi	3.26 (2)
PB1—O23^vii	2.532 (15)	O22—PB1^viii	4.49 (2)
PB1—O1^ii	3.121 (19)	O22—PB1^ix	2.595 (18)
PB1—O1^iii	3.22 (2)	O22—PB2^x	2.519 (19)
PB1—O1^iv	3.121 (19)	O22—PB2^xii	2.81 (2)
PB1—O1^v	3.22 (2)	O22—PB2^viii	4.478 (18)
PB1—O1^vi	3.175 (16)	O22—PB2^ix	3.034 (12)
PB1—O1^vii	3.175 (16)	O22—P	1.524 (9)
PB2—PB1	4.239 (5)	O22—P^xv	4.447 (12)
PB2—PB1^viii	4.148 (18)	O22—P^x	4.237 (17)
PB2—PB1^ix	3.829 (16)	O22—P^xii	4.318 (19)
PB2—PB1^vi	4.085 (11)	O22—P^xx	4.216 (11)
PB2—PB2^iv	3.565 (11)	O22—P^xiv	3.719 (17)
PB2—PB2^v	3.565 (11)	O22—O21	2.505 (10)
PB2—PB2^vi	3.80 (2)	O22—O21^xv	3.030 (10)
PB2—P	3.859 (7)	O22—O21^xxiii	4.371 (14)
PB2—P^x	3.242 (16)	O22—O21^xiv	3.215 (19)
PB2—P^xi	3.676 (12)	O22—O22^x	4.16 (3)
PB2—P^xii	3.137 (14)	O22—O22^xiv	4.11 (3)
PB2—P^ii	4.426 (11)	O22—O22^xxiv	4.45 (3)
PB2—P^iii	4.170 (12)	O22—O23	2.491 (10)
PB2—P^vii	4.196 (12)	O22—O23^xii	4.135 (18)
PB2—O21^x	2.92 (2)	O22—O23^xx	2.823 (14)
PB2—O21^xi	2.96 (2)	O22—O23^xiv	3.285 (19)
PB2—O21^xii	4.429 (16)	O22—O1	2.480 (9)
PB2—O21^iii	2.841 (15)	O22—O1^x	3.165 (16)
PB2—O21^vii	4.481 (18)	O22—O1^xii	3.31 (2)
PB2—O22^x	2.519 (19)	O23—PB1^ix	4.425 (16)
PB2—O22^xii	2.81 (2)	O23—PB1^vi	2.532 (15)
PB2—O22^ii	3.034 (12)	O23—PB2^xi	3.251 (14)
PB2—O22^iii	4.478 (18)	O23—PB2^xii	2.420 (14)
PB2—O23^xi	3.251 (14)	O23—PB2^xiii	2.897 (13)
PB2—O23^xii	2.420 (14)	O23—P	1.527 (9)
PB2—O23^vii	2.897 (13)	O23—P^xi	4.422 (17)
PB2—O1	2.348 (8)	O23—P^xii	4.128 (17)
PB2—O1^x	3.985 (18)	O23—P^xvi	4.458 (16)
PB2—O1^xi	4.395 (15)	O23—P^xviii	4.167 (14)
PB2—O1^xii	3.922 (16)	O23—P^xiv	3.734 (17)
P—PB1^viii	3.493 (16)	O23—O21	2.507 (9)
P—PB1^ix	3.445 (15)	O23—O21^xi	4.185 (19)
P—PB1^vi	3.435 (8)	O23—O21^xvi	3.130 (17)
P—PB2	3.859 (7)	O23—O21^xiv	3.232 (19)
P—PB2^x	3.242 (16)	O23—O22	2.491 (10)
P—PB2^xi	3.676 (12)	O23—O22^xii	4.135 (18)
P—PB2^xii	3.137 (14)	O23—O22^xviii	2.823 (14)
P—PB2^viii	4.170 (12)	O23—O22^xiv	3.285 (19)
P—PB2^ix	4.426 (11)	O23—O23^xxv	4.447 (17)
P—PB2^xiii	4.196 (12)	O23—O23^xxvi	4.447 (17)
P—P^x	4.199 (14)	O23—O23^xiv	4.14 (3)
P—P^xi	4.303 (14)	O23—O1	2.482 (9)
P—P^xii	4.129 (16)	O23—O1^xi	3.48 (2)
P—P^xiv	3.927 (8)	O23—O1^xii	3.060 (18)
P—O21	1.544 (9)	O1—PB1^viii	3.22 (2)
P—O21^xv	4.283 (11)	O1—PB1^ix	3.121 (19)
P—O21^x	4.344 (17)	O1—PB1^vi	3.175 (16)
P—O21^xi	4.25 (2)	O1—PB2	2.348 (8)
P—O21^xvi	4.413 (12)	O1—PB2^x	3.985 (18)
P—O21^xiv	3.674 (17)	O1—PB2^xi	4.395 (15)
P—O22^xvii	4.447 (12)	O1—PB2^xii	3.922 (16)
P—O22	1.524 (9)	O1—P	1.513 (7)
P—O22^x	4.237 (17)	O1—P^x	3.37 (2)
P—O22^xii	4.318 (19)	O1—P^xi	3.556 (19)
P—O22^xviii	4.216 (11)	O1—P^xii	3.30 (2)
P—O22^xiv	3.719 (17)	O1—O21	2.496 (9)
P—O23	1.527 (9)	O1—O21^x	3.340 (16)
P—O23^xi	4.422 (17)	O1—O21^xi	3.26 (2)
P—O23^xii	4.128 (17)	O1—O22	2.480 (9)
P—O23^xix	4.458 (16)	O1—O22^x	3.165 (16)
P—O23^xx	4.167 (14)	O1—O22^xii	3.31 (2)
P—O23^xiv	3.734 (17)	O1—O23	2.482 (9)
P—O1	1.513 (7)	O1—O23^xi	3.48 (2)
P—O1^x	3.37 (2)	O1—O23^xii	3.060 (18)
P—O1^xi	3.556 (19)	O1—O1^x	3.11 (3)
P—O1^xii	3.30 (2)	O1—O1^xi	3.37 (3)
O21—PB1^viii	2.581 (18)	O1—O1^xii	3.06 (3)
O21—PB1^vi	4.387 (14)
O21—P—O22	109.45 (14)	O22—P—O23	109.45 (12)
O21—P—O23	109.45 (12)	O22—P—O1	109.48 (13)
O21—P—O1	109.50 (13)	O23—P—O1	109.50 (13)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, y−1, z; (xviii) x, −y+1, z+3/2; (xix) x, −y, z+1/2; (xx) x, −y+1, z+1/2; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2; (xxiv) −x+3/2, −y+3/2, −z+1; (xxv) −x+3/2, y−1/2, −z+3/2; (xxvi) −x+3/2, y+1/2, −z+3/2.

(S2P14_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8978 (9) Å	T = 298 K
c = 2.8306 (14) Å	Particle morphology: Pressure cell anvil material
V = 20.59 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.586 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.63 Angstrom (no useful data)
Rp = 0.077	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 86.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 121.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 281.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.061	50 parameters
Rexp = 0.062	10 restraints
R(F^2) = 0.16735	(Δ/σ)max < 0.001
χ^2 = 0.980	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.121031 2: -4.985370E-02 3: 8.278980E-02 4: -4.438680E-02 5: 3.960540E-02 6: -3.841700E-02 7: 2.405080E-02 8: -2.353800E-02 9: 1.616540E-0210: -1.192490E-0211: 3.316930E-0312: -2.329230E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89802 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.239 (5)	O21—PB2^ii	2.92 (2)
PB1—PB2^i	4.239 (5)	O21—PB2	2.96 (2)
PB1—PB2	3.829 (16)	O21—PB2	4.429 (16)
PB1—PB2	4.148 (18)	O21—PB2	2.841 (15)
PB1—PB2	3.829 (16)	O21—PB2	4.481 (18)
PB1—PB2	4.148 (18)	O21—P^iv	4.283 (11)
PB1—PB2	4.085 (11)	O21—P	1.544 (9)
PB1—PB2	4.085 (11)	O21—P^ii	4.344 (17)
PB1—P	3.445 (15)	O21—P	4.25 (2)
PB1—P	3.493 (16)	O21—P	4.413 (12)
PB1—P	3.445 (15)	O21—P	3.674 (17)
PB1—P	3.493 (16)	O21—O21^ii	4.24 (3)
PB1—P	3.435 (8)	O21—O21	4.39 (3)
PB1—P	3.435 (8)	O21—O21	4.04 (3)
PB1—O21	2.581 (18)	O21—O22^iv	3.030 (10)
PB1—O21	2.581 (18)	O21—O22	2.505 (10)
PB1—O21	4.387 (14)	O21—O22	4.371 (14)
PB1—O21	4.387 (14)	O21—O22	3.215 (19)
PB1—O22	2.595 (18)	O21—O23	2.507 (9)
PB1—O22	4.49 (2)	O21—O23	4.185 (19)
PB1—O22	2.595 (18)	O21—O23	3.130 (17)
PB1—O22	4.49 (2)	O21—O23	3.232 (19)
PB1—O23	4.425 (16)	O21—O1	2.496 (9)
PB1—O23	4.425 (16)	O21—O1^ii	3.340 (16)
PB1—O23	2.532 (15)	O21—O1	3.26 (2)
PB1—O23	2.532 (15)	O22—PB1	4.49 (2)
PB1—O1	3.121 (19)	O22—PB1	2.595 (18)
PB1—O1	3.22 (2)	O22—PB2^ii	2.519 (19)
PB1—O1	3.121 (19)	O22—PB2	2.81 (2)
PB1—O1	3.22 (2)	O22—PB2	4.478 (18)
PB1—O1	3.175 (16)	O22—PB2	3.034 (12)
PB1—O1	3.175 (16)	O22—P	1.524 (9)
PB2—PB1	4.239 (5)	O22—P^iii	4.447 (12)
PB2—PB1	4.148 (18)	O22—P^ii	4.237 (17)
PB2—PB1	3.829 (16)	O22—P	4.318 (19)
PB2—PB1	4.085 (11)	O22—P	4.216 (11)
PB2—PB2	3.565 (11)	O22—P	3.719 (17)
PB2—PB2	3.565 (11)	O22—O21	2.505 (10)
PB2—PB2	3.80 (2)	O22—O21^iii	3.030 (10)
PB2—P	3.859 (7)	O22—O21	4.371 (14)
PB2—P^ii	3.242 (16)	O22—O21	3.215 (19)
PB2—P	3.676 (12)	O22—O22^ii	4.16 (3)
PB2—P	3.137 (14)	O22—O22	4.11 (3)
PB2—P	4.426 (11)	O22—O22	4.45 (3)
PB2—P	4.170 (12)	O22—O23	2.491 (10)
PB2—P	4.196 (12)	O22—O23	4.135 (18)
PB2—O21^ii	2.92 (2)	O22—O23	2.823 (14)
PB2—O21	2.96 (2)	O22—O23	3.285 (19)
PB2—O21	4.429 (16)	O22—O1	2.480 (9)
PB2—O21	2.841 (15)	O22—O1^ii	3.165 (16)
PB2—O21	4.481 (18)	O22—O1	3.31 (2)
PB2—O22^ii	2.519 (19)	O23—PB1	4.425 (16)
PB2—O22	2.81 (2)	O23—PB1	2.532 (15)
PB2—O22	3.034 (12)	O23—PB2	3.251 (14)
PB2—O22	4.478 (18)	O23—PB2	2.420 (14)
PB2—O23	3.251 (14)	O23—PB2	2.897 (13)
PB2—O23	2.420 (14)	O23—P	1.527 (9)
PB2—O23	2.897 (13)	O23—P	4.422 (17)
PB2—O1	2.348 (8)	O23—P	4.128 (17)
PB2—O1^ii	3.985 (18)	O23—P	4.458 (16)
PB2—O1	4.395 (15)	O23—P	4.167 (14)
PB2—O1	3.922 (16)	O23—P	3.734 (17)
P—PB1	3.493 (16)	O23—O21	2.507 (9)
P—PB1	3.445 (15)	O23—O21	4.185 (19)
P—PB1	3.435 (8)	O23—O21	3.130 (17)
P—PB2	3.859 (7)	O23—O21	3.232 (19)
P—PB2^ii	3.242 (16)	O23—O22	2.491 (10)
P—PB2	3.676 (12)	O23—O22	4.135 (18)
P—PB2	3.137 (14)	O23—O22	2.823 (14)
P—PB2	4.170 (12)	O23—O22	3.285 (19)
P—PB2	4.426 (11)	O23—O23	4.447 (17)
P—PB2	4.196 (12)	O23—O23	4.447 (17)
P—P^ii	4.199 (14)	O23—O23	4.14 (3)
P—P	4.303 (14)	O23—O1	2.482 (9)
P—P	4.129 (16)	O23—O1	3.48 (2)
P—P	3.927 (8)	O23—O1	3.060 (18)
P—O21	1.544 (9)	O1—PB1	3.22 (2)
P—O21^iii	4.283 (11)	O1—PB1	3.121 (19)
P—O21^ii	4.344 (17)	O1—PB1	3.175 (16)
P—O21	4.25 (2)	O1—PB2	2.348 (8)
P—O21	4.413 (12)	O1—PB2^ii	3.985 (18)
P—O21	3.674 (17)	O1—PB2	4.395 (15)
P—O22^iv	4.447 (12)	O1—PB2	3.922 (16)
P—O22	1.524 (9)	O1—P	1.513 (7)
P—O22^ii	4.237 (17)	O1—P^ii	3.37 (2)
P—O22	4.318 (19)	O1—P	3.556 (19)
P—O22	4.216 (11)	O1—P	3.30 (2)
P—O22	3.719 (17)	O1—O21	2.496 (9)
P—O23	1.527 (9)	O1—O21^ii	3.340 (16)
P—O23	4.422 (17)	O1—O21	3.26 (2)
P—O23	4.128 (17)	O1—O22	2.480 (9)
P—O23	4.458 (16)	O1—O22^ii	3.165 (16)
P—O23	4.167 (14)	O1—O22	3.31 (2)
P—O23	3.734 (17)	O1—O23	2.482 (9)
P—O1	1.513 (7)	O1—O23	3.48 (2)
P—O1^ii	3.37 (2)	O1—O23	3.060 (18)
P—O1	3.556 (19)	O1—O1^ii	3.11 (3)
P—O1	3.30 (2)	O1—O1	3.37 (3)
O21—PB1	2.581 (18)	O1—O1	3.06 (3)
O21—PB1	4.387 (14)
O21—P—O22	109.45 (14)	O22—P—O23	109.45 (12)
O21—P—O23	109.45 (12)	O22—P—O1	109.48 (13)
O21—P—O1	109.50 (13)	O23—P—O1	109.50 (13)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(S2P14_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5560 (8) Å	Particle morphology: Component of pressure cell, not sample
V = 44.96 (4) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.586 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.63 Angstrom (no useful data)
Rp = 0.077	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 86.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 121.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 281.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.061	50 parameters
Rexp = 0.062	10 restraints
R(F^2) = 0.16735	(Δ/σ)max < 0.001
χ^2 = 0.980	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.121031 2: -4.985370E-02 3: 8.278980E-02 4: -4.438680E-02 5: 3.960540E-02 6: -3.841700E-02 7: 2.405080E-02 8: -2.353800E-02 9: 1.616540E-0210: -1.192490E-0211: 3.316930E-0312: -2.329230E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89802 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.239 (5)	O21—PB2^x	2.92 (2)
PB1—PB2^i	4.239 (5)	O21—PB2^xi	2.96 (2)
PB1—PB2^ii	3.829 (16)	O21—PB2^xii	4.429 (16)
PB1—PB2^iii	4.148 (18)	O21—PB2^viii	2.841 (15)
PB1—PB2^iv	3.829 (16)	O21—PB2^xiii	4.481 (18)
PB1—PB2^v	4.148 (18)	O21—P^xvii	4.283 (11)
PB1—PB2^vi	4.085 (11)	O21—P	1.544 (9)
PB1—PB2^vii	4.085 (11)	O21—P^x	4.344 (17)
PB1—P^ii	3.445 (15)	O21—P^xi	4.25 (2)
PB1—P^iii	3.493 (16)	O21—P^xix	4.413 (12)
PB1—P^iv	3.445 (15)	O21—P^xiv	3.674 (17)
PB1—P^v	3.493 (16)	O21—O21^x	4.24 (3)
PB1—P^vi	3.435 (8)	O21—O21^xxi	4.39 (3)
PB1—P^vii	3.435 (8)	O21—O21^xiv	4.04 (3)
PB1—O21^iii	2.581 (18)	O21—O22^xvii	3.030 (10)
PB1—O21^v	2.581 (18)	O21—O22	2.505 (10)
PB1—O21^vi	4.387 (14)	O21—O22^xxii	4.371 (14)
PB1—O21^vii	4.387 (14)	O21—O22^xiv	3.215 (19)
PB1—O22^ii	2.595 (18)	O21—O23	2.507 (9)
PB1—O22^iii	4.49 (2)	O21—O23^xi	4.185 (19)
PB1—O22^iv	2.595 (18)	O21—O23^xix	3.130 (17)
PB1—O22^v	4.49 (2)	O21—O23^xiv	3.232 (19)
PB1—O23^ii	4.425 (16)	O21—O1	2.496 (9)
PB1—O23^iv	4.425 (16)	O21—O1^x	3.340 (16)
PB1—O23^vi	2.532 (15)	O21—O1^xi	3.26 (2)
PB1—O23^vii	2.532 (15)	O22—PB1^viii	4.49 (2)
PB1—O1^ii	3.121 (19)	O22—PB1^ix	2.595 (18)
PB1—O1^iii	3.22 (2)	O22—PB2^x	2.519 (19)
PB1—O1^iv	3.121 (19)	O22—PB2^xii	2.81 (2)
PB1—O1^v	3.22 (2)	O22—PB2^viii	4.478 (18)
PB1—O1^vi	3.175 (16)	O22—PB2^ix	3.034 (12)
PB1—O1^vii	3.175 (16)	O22—P	1.524 (9)
PB2—PB1	4.239 (5)	O22—P^xv	4.447 (12)
PB2—PB1^viii	4.148 (18)	O22—P^x	4.237 (17)
PB2—PB1^ix	3.829 (16)	O22—P^xii	4.318 (19)
PB2—PB1^vi	4.085 (11)	O22—P^xx	4.216 (11)
PB2—PB2^iv	3.565 (11)	O22—P^xiv	3.719 (17)
PB2—PB2^v	3.565 (11)	O22—O21	2.505 (10)
PB2—PB2^vi	3.80 (2)	O22—O21^xv	3.030 (10)
PB2—P	3.859 (7)	O22—O21^xxiii	4.371 (14)
PB2—P^x	3.242 (16)	O22—O21^xiv	3.215 (19)
PB2—P^xi	3.676 (12)	O22—O22^x	4.16 (3)
PB2—P^xii	3.137 (14)	O22—O22^xiv	4.11 (3)
PB2—P^ii	4.426 (11)	O22—O22^xxiv	4.45 (3)
PB2—P^iii	4.170 (12)	O22—O23	2.491 (10)
PB2—P^vii	4.196 (12)	O22—O23^xii	4.135 (18)
PB2—O21^x	2.92 (2)	O22—O23^xx	2.823 (14)
PB2—O21^xi	2.96 (2)	O22—O23^xiv	3.285 (19)
PB2—O21^xii	4.429 (16)	O22—O1	2.480 (9)
PB2—O21^iii	2.841 (15)	O22—O1^x	3.165 (16)
PB2—O21^vii	4.481 (18)	O22—O1^xii	3.31 (2)
PB2—O22^x	2.519 (19)	O23—PB1^ix	4.425 (16)
PB2—O22^xii	2.81 (2)	O23—PB1^vi	2.532 (15)
PB2—O22^ii	3.034 (12)	O23—PB2^xi	3.251 (14)
PB2—O22^iii	4.478 (18)	O23—PB2^xii	2.420 (14)
PB2—O23^xi	3.251 (14)	O23—PB2^xiii	2.897 (13)
PB2—O23^xii	2.420 (14)	O23—P	1.527 (9)
PB2—O23^vii	2.897 (13)	O23—P^xi	4.422 (17)
PB2—O1	2.348 (8)	O23—P^xii	4.128 (17)
PB2—O1^x	3.985 (18)	O23—P^xvi	4.458 (16)
PB2—O1^xi	4.395 (15)	O23—P^xviii	4.167 (14)
PB2—O1^xii	3.922 (16)	O23—P^xiv	3.734 (17)
P—PB1^viii	3.493 (16)	O23—O21	2.507 (9)
P—PB1^ix	3.445 (15)	O23—O21^xi	4.185 (19)
P—PB1^vi	3.435 (8)	O23—O21^xvi	3.130 (17)
P—PB2	3.859 (7)	O23—O21^xiv	3.232 (19)
P—PB2^x	3.242 (16)	O23—O22	2.491 (10)
P—PB2^xi	3.676 (12)	O23—O22^xii	4.135 (18)
P—PB2^xii	3.137 (14)	O23—O22^xviii	2.823 (14)
P—PB2^viii	4.170 (12)	O23—O22^xiv	3.285 (19)
P—PB2^ix	4.426 (11)	O23—O23^xxv	4.447 (17)
P—PB2^xiii	4.196 (12)	O23—O23^xxvi	4.447 (17)
P—P^x	4.199 (14)	O23—O23^xiv	4.14 (3)
P—P^xi	4.303 (14)	O23—O1	2.482 (9)
P—P^xii	4.129 (16)	O23—O1^xi	3.48 (2)
P—P^xiv	3.927 (8)	O23—O1^xii	3.060 (18)
P—O21	1.544 (9)	O1—PB1^viii	3.22 (2)
P—O21^xv	4.283 (11)	O1—PB1^ix	3.121 (19)
P—O21^x	4.344 (17)	O1—PB1^vi	3.175 (16)
P—O21^xi	4.25 (2)	O1—PB2	2.348 (8)
P—O21^xvi	4.413 (12)	O1—PB2^x	3.985 (18)
P—O21^xiv	3.674 (17)	O1—PB2^xi	4.395 (15)
P—O22^xvii	4.447 (12)	O1—PB2^xii	3.922 (16)
P—O22	1.524 (9)	O1—P	1.513 (7)
P—O22^x	4.237 (17)	O1—P^x	3.37 (2)
P—O22^xii	4.318 (19)	O1—P^xi	3.556 (19)
P—O22^xviii	4.216 (11)	O1—P^xii	3.30 (2)
P—O22^xiv	3.719 (17)	O1—O21	2.496 (9)
P—O23	1.527 (9)	O1—O21^x	3.340 (16)
P—O23^xi	4.422 (17)	O1—O21^xi	3.26 (2)
P—O23^xii	4.128 (17)	O1—O22	2.480 (9)
P—O23^xix	4.458 (16)	O1—O22^x	3.165 (16)
P—O23^xx	4.167 (14)	O1—O22^xii	3.31 (2)
P—O23^xiv	3.734 (17)	O1—O23	2.482 (9)
P—O1	1.513 (7)	O1—O23^xi	3.48 (2)
P—O1^x	3.37 (2)	O1—O23^xii	3.060 (18)
P—O1^xi	3.556 (19)	O1—O1^x	3.11 (3)
P—O1^xii	3.30 (2)	O1—O1^xi	3.37 (3)
O21—PB1^viii	2.581 (18)	O1—O1^xii	3.06 (3)
O21—PB1^vi	4.387 (14)
O21—P—O22	109.45 (14)	O22—P—O23	109.45 (12)
O21—P—O23	109.45 (12)	O22—P—O1	109.48 (13)
O21—P—O1	109.50 (13)	O23—P—O1	109.50 (13)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) x, y+1, z; (xvi) −z, −x, −y+1; (xvii) x, y−1, z; (xviii) −z, −x+1, −y+1; (xix) −z, −x, −y; (xx) −z, −x+1, −y; (xxi) −x+1, −y−1/2, −z+3/2; (xxii) z+1, x−1/2, y+1/2; (xxiii) z+1, x+1/2, y+1/2; (xxiv) −x+1, −y+3/2, −z+3/2; (xxv) z+1, x−1/2, y+3/2; (xxvi) z+1, x+1/2, y+3/2.

(S2P16_phase_1)

Crystal data

O8P2Pb3	V = 694.96 (12) Å^3
Mr = 811.74	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7473 (14) Å	T = 298 K
b = 5.5007 (8) Å	Particle morphology: plate
c = 9.4358 (12) Å	irregular, 6 × 6 mm
β = 103.104 (16)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.083	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 86.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 110.5 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 228.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.064	48 parameters
Rexp = 0.065	10 restraints
R(F^2) = 0.18021	(Δ/σ)max = 0.03
χ^2 = 1.000	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 8.256520E-02 2: 6.523940E-03 3: 2.208510E-02 4: 2.331650E-04 5: -5.602230E-03 6: -6.446600E-03 7: -5.068810E-03 8: -6.062250E-03 9: 3.249320E-0310: -7.517300E-0311: 1.452010E-0312: -2.585640E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.88185 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
PB1	0.0	0.259 (4)	0.25	0.028 (2)*
PB2	0.3157 (4)	0.283 (3)	0.3480 (18)	0.028 (2)*
P	0.6038 (3)	0.258 (2)	0.4556 (10)	0.013 (2)*
O21	0.6398 (10)	0.014 (3)	0.4051 (15)	0.0124 (16)*
O22	0.6479 (9)	0.467 (3)	0.3848 (15)	0.0124 (16)*
O23	0.6379 (10)	0.278 (3)	0.6211 (12)	0.0124 (16)*
O1	0.4914 (4)	0.270 (3)	0.4120 (19)	0.0124 (16)*

Geometric parameters (Å, º)

PB1—PB2	4.230 (5)	O21—PB2^x	2.99 (2)
PB1—PB2^i	4.230 (5)	O21—PB2^xi	2.80 (2)
PB1—PB2^ii	3.90 (2)	O21—PB2^xii	4.49 (2)
PB1—PB2^iii	4.08 (2)	O21—PB2^viii	2.890 (18)
PB1—PB2^iv	3.90 (2)	O21—PB2^xiii	4.470 (19)
PB1—PB2^v	4.08 (2)	O21—P^xvii	4.227 (10)
PB1—PB2^vi	4.062 (14)	O21—P	1.543 (8)
PB1—PB2^vii	4.062 (14)	O21—P^x	4.408 (17)
PB1—P^ii	3.485 (19)	O21—P^xi	4.14 (2)
PB1—P^iii	3.48 (2)	O21—P^xix	4.418 (12)
PB1—P^iv	3.485 (19)	O21—P^xiv	3.692 (18)
PB1—P^v	3.48 (2)	O21—O21^x	4.27 (3)
PB1—P^vi	3.400 (9)	O21—O21^xxi	4.29 (3)
PB1—P^vii	3.400 (9)	O21—O21^xiv	4.08 (3)
PB1—O21^iii	2.55 (2)	O21—O22^xvii	3.020 (10)
PB1—O21^v	2.55 (2)	O21—O22	2.503 (9)
PB1—O21^vi	4.321 (14)	O21—O22^xxii	4.437 (16)
PB1—O21^vii	4.321 (14)	O21—O22^xiv	3.137 (18)
PB1—O22^ii	2.68 (2)	O21—O23	2.508 (9)
PB1—O22^iii	4.44 (2)	O21—O23^xi	4.097 (18)
PB1—O22^iv	2.68 (2)	O21—O23^xix	3.120 (18)
PB1—O22^v	4.44 (2)	O21—O23^xiv	3.325 (19)
PB1—O23^ii	4.455 (18)	O21—O1	2.491 (9)
PB1—O23^iv	4.455 (18)	O21—O1^x	3.426 (16)
PB1—O23^vi	2.482 (14)	O21—O1^xi	3.18 (2)
PB1—O23^vii	2.482 (14)	O22—PB1^viii	4.44 (2)
PB1—O1^ii	3.11 (2)	O22—PB1^ix	2.68 (2)
PB1—O1^iii	3.21 (2)	O22—PB2^x	2.57 (2)
PB1—O1^iv	3.11 (2)	O22—PB2^xii	2.82 (3)
PB1—O1^v	3.21 (2)	O22—PB2^viii	4.469 (18)
PB1—O1^vi	3.169 (18)	O22—PB2^ix	2.970 (15)
PB1—O1^vii	3.169 (18)	O22—P	1.522 (9)
PB2—PB1	4.230 (5)	O22—P^xv	4.465 (11)
PB2—PB1^viii	4.08 (2)	O22—P^x	4.309 (17)
PB2—PB1^ix	3.90 (2)	O22—P^xii	4.346 (19)
PB2—PB1^vi	4.062 (14)	O22—P^xx	4.236 (11)
PB2—PB2^iv	3.569 (14)	O22—P^xiv	3.622 (16)
PB2—PB2^v	3.569 (14)	O22—O21	2.503 (9)
PB2—PB2^vi	3.74 (3)	O22—O21^xv	3.020 (10)
PB2—P	3.861 (7)	O22—O21^xxiii	4.437 (16)
PB2—P^x	3.30 (2)	O22—O21^xiv	3.137 (18)
PB2—P^xi	3.546 (17)	O22—O22^x	4.28 (2)
PB2—P^xii	3.180 (18)	O22—O22^xiv	3.94 (3)
PB2—P^ii	4.380 (14)	O22—O22^xxiv	4.42 (3)
PB2—P^iii	4.207 (15)	O22—O23	2.492 (10)
PB2—P^vii	4.166 (13)	O22—O23^xii	4.160 (18)
PB2—O21^x	2.99 (2)	O22—O23^xx	2.831 (16)
PB2—O21^xi	2.80 (2)	O22—O23^xiv	3.251 (19)
PB2—O21^xii	4.49 (2)	O22—O1	2.474 (9)
PB2—O21^iii	2.890 (18)	O22—O1^x	3.201 (17)
PB2—O21^vii	4.470 (19)	O22—O1^xii	3.33 (2)
PB2—O22^x	2.57 (2)	O23—PB1^ix	4.455 (18)
PB2—O22^xii	2.82 (3)	O23—PB1^vi	2.482 (14)
PB2—O22^ii	2.970 (15)	O23—PB2^xi	3.151 (18)
PB2—O22^iii	4.469 (18)	O23—PB2^xii	2.498 (18)
PB2—O23^xi	3.151 (18)	O23—PB2^xiii	2.881 (15)
PB2—O23^xii	2.498 (18)	O23—P	1.529 (9)
PB2—O23^vii	2.881 (15)	O23—P^xi	4.379 (18)
PB2—O1	2.353 (8)	O23—P^xii	4.120 (18)
PB2—O1^x	4.00 (2)	O23—P^xvi	4.422 (17)
PB2—O1^xi	4.322 (16)	O23—P^xviii	4.166 (16)
PB2—O1^xii	3.937 (18)	O23—P^xiv	3.787 (16)
P—PB1^viii	3.48 (2)	O23—O21	2.508 (9)
P—PB1^ix	3.485 (19)	O23—O21^xi	4.097 (18)
P—PB1^vi	3.400 (9)	O23—O21^xvi	3.120 (18)
P—PB2	3.861 (7)	O23—O21^xiv	3.325 (19)
P—PB2^x	3.30 (2)	O23—O22	2.492 (10)
P—PB2^xi	3.546 (17)	O23—O22^xii	4.160 (18)
P—PB2^xii	3.180 (18)	O23—O22^xviii	2.831 (16)
P—PB2^viii	4.207 (15)	O23—O22^xiv	3.251 (19)
P—PB2^ix	4.380 (14)	O23—O23^xxv	4.425 (18)
P—PB2^xiii	4.166 (13)	O23—O23^xxvi	4.425 (18)
P—P^x	4.264 (15)	O23—O23^xiv	4.25 (3)
P—P^xi	4.241 (17)	O23—O1	2.480 (9)
P—P^xii	4.124 (17)	O23—O1^xi	3.48 (2)
P—P^xiv	3.917 (8)	O23—O1^xii	3.03 (2)
P—O21	1.543 (8)	O1—PB1^viii	3.21 (2)
P—O21^xv	4.227 (10)	O1—PB1^ix	3.11 (2)
P—O21^x	4.408 (17)	O1—PB1^vi	3.169 (18)
P—O21^xi	4.14 (2)	O1—PB2	2.353 (8)
P—O21^xvi	4.418 (12)	O1—PB2^x	4.00 (2)
P—O21^xiv	3.692 (18)	O1—PB2^xi	4.322 (16)
P—O22^xvii	4.465 (11)	O1—PB2^xii	3.937 (18)
P—O22	1.522 (9)	O1—P	1.508 (6)
P—O22^x	4.309 (17)	O1—P^x	3.42 (2)
P—O22^xii	4.346 (19)	O1—P^xi	3.53 (2)
P—O22^xviii	4.236 (11)	O1—P^xii	3.28 (2)
P—O22^xiv	3.622 (16)	O1—O21	2.491 (9)
P—O23	1.529 (9)	O1—O21^x	3.426 (16)
P—O23^xi	4.379 (18)	O1—O21^xi	3.18 (2)
P—O23^xii	4.120 (18)	O1—O22	2.474 (9)
P—O23^xix	4.422 (17)	O1—O22^x	3.201 (17)
P—O23^xx	4.166 (16)	O1—O22^xii	3.33 (2)
P—O23^xiv	3.787 (16)	O1—O23	2.480 (9)
P—O1	1.508 (6)	O1—O23^xi	3.48 (2)
P—O1^x	3.42 (2)	O1—O23^xii	3.03 (2)
P—O1^xi	3.53 (2)	O1—O1^x	3.12 (4)
P—O1^xii	3.28 (2)	O1—O1^xi	3.38 (3)
O21—PB1^viii	2.55 (2)	O1—O1^xii	3.01 (3)
O21—PB1^vi	4.321 (14)
O21—P—O22	109.47 (14)	O22—P—O23	109.45 (12)
O21—P—O23	109.46 (12)	O22—P—O1	109.47 (13)
O21—P—O1	109.48 (13)	O23—P—O1	109.50 (13)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, y−1, z; (xviii) x, −y+1, z+3/2; (xix) x, −y, z+1/2; (xx) x, −y+1, z+1/2; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2; (xxiv) −x+3/2, −y+3/2, −z+1; (xxv) −x+3/2, y−1/2, −z+3/2; (xxvi) −x+3/2, y+1/2, −z+3/2.

(S2P16_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8990 (9) Å	T = 298 K
c = 2.8304 (13) Å	Particle morphology: Pressure cell anvil material
V = 20.60 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.083	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 86.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 110.5 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 228.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.064	48 parameters
Rexp = 0.065	10 restraints
R(F^2) = 0.18021	(Δ/σ)max = 0.03
χ^2 = 1.000	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 8.256520E-02 2: 6.523940E-03 3: 2.208510E-02 4: 2.331650E-04 5: -5.602230E-03 6: -6.446600E-03 7: -5.068810E-03 8: -6.062250E-03 9: 3.249320E-0310: -7.517300E-0311: 1.452010E-0312: -2.585640E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.88185 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.230 (5)	O21—PB2^ii	2.99 (2)
PB1—PB2^i	4.230 (5)	O21—PB2	2.80 (2)
PB1—PB2	3.90 (2)	O21—PB2	4.49 (2)
PB1—PB2	4.08 (2)	O21—PB2	2.890 (18)
PB1—PB2	3.90 (2)	O21—PB2	4.470 (19)
PB1—PB2	4.08 (2)	O21—P^iv	4.227 (10)
PB1—PB2	4.062 (14)	O21—P	1.543 (8)
PB1—PB2	4.062 (14)	O21—P^ii	4.408 (17)
PB1—P	3.485 (19)	O21—P	4.14 (2)
PB1—P	3.48 (2)	O21—P	4.418 (12)
PB1—P	3.485 (19)	O21—P	3.692 (18)
PB1—P	3.48 (2)	O21—O21^ii	4.27 (3)
PB1—P	3.400 (9)	O21—O21	4.29 (3)
PB1—P	3.400 (9)	O21—O21	4.08 (3)
PB1—O21	2.55 (2)	O21—O22^iv	3.020 (10)
PB1—O21	2.55 (2)	O21—O22	2.503 (9)
PB1—O21	4.321 (14)	O21—O22	4.437 (16)
PB1—O21	4.321 (14)	O21—O22	3.137 (18)
PB1—O22	2.68 (2)	O21—O23	2.508 (9)
PB1—O22	4.44 (2)	O21—O23	4.097 (18)
PB1—O22	2.68 (2)	O21—O23	3.120 (18)
PB1—O22	4.44 (2)	O21—O23	3.325 (19)
PB1—O23	4.455 (18)	O21—O1	2.491 (9)
PB1—O23	4.455 (18)	O21—O1^ii	3.426 (16)
PB1—O23	2.482 (14)	O21—O1	3.18 (2)
PB1—O23	2.482 (14)	O22—PB1	4.44 (2)
PB1—O1	3.11 (2)	O22—PB1	2.68 (2)
PB1—O1	3.21 (2)	O22—PB2^ii	2.57 (2)
PB1—O1	3.11 (2)	O22—PB2	2.82 (3)
PB1—O1	3.21 (2)	O22—PB2	4.469 (18)
PB1—O1	3.169 (18)	O22—PB2	2.970 (15)
PB1—O1	3.169 (18)	O22—P	1.522 (9)
PB2—PB1	4.230 (5)	O22—P^iii	4.465 (11)
PB2—PB1	4.08 (2)	O22—P^ii	4.309 (17)
PB2—PB1	3.90 (2)	O22—P	4.346 (19)
PB2—PB1	4.062 (14)	O22—P	4.236 (11)
PB2—PB2	3.569 (14)	O22—P	3.622 (16)
PB2—PB2	3.569 (14)	O22—O21	2.503 (9)
PB2—PB2	3.74 (3)	O22—O21^iii	3.020 (10)
PB2—P	3.861 (7)	O22—O21	4.437 (16)
PB2—P^ii	3.30 (2)	O22—O21	3.137 (18)
PB2—P	3.546 (17)	O22—O22^ii	4.28 (2)
PB2—P	3.180 (18)	O22—O22	3.94 (3)
PB2—P	4.380 (14)	O22—O22	4.42 (3)
PB2—P	4.207 (15)	O22—O23	2.492 (10)
PB2—P	4.166 (13)	O22—O23	4.160 (18)
PB2—O21^ii	2.99 (2)	O22—O23	2.831 (16)
PB2—O21	2.80 (2)	O22—O23	3.251 (19)
PB2—O21	4.49 (2)	O22—O1	2.474 (9)
PB2—O21	2.890 (18)	O22—O1^ii	3.201 (17)
PB2—O21	4.470 (19)	O22—O1	3.33 (2)
PB2—O22^ii	2.57 (2)	O23—PB1	4.455 (18)
PB2—O22	2.82 (3)	O23—PB1	2.482 (14)
PB2—O22	2.970 (15)	O23—PB2	3.151 (18)
PB2—O22	4.469 (18)	O23—PB2	2.498 (18)
PB2—O23	3.151 (18)	O23—PB2	2.881 (15)
PB2—O23	2.498 (18)	O23—P	1.529 (9)
PB2—O23	2.881 (15)	O23—P	4.379 (18)
PB2—O1	2.353 (8)	O23—P	4.120 (18)
PB2—O1^ii	4.00 (2)	O23—P	4.422 (17)
PB2—O1	4.322 (16)	O23—P	4.166 (16)
PB2—O1	3.937 (18)	O23—P	3.787 (16)
P—PB1	3.48 (2)	O23—O21	2.508 (9)
P—PB1	3.485 (19)	O23—O21	4.097 (18)
P—PB1	3.400 (9)	O23—O21	3.120 (18)
P—PB2	3.861 (7)	O23—O21	3.325 (19)
P—PB2^ii	3.30 (2)	O23—O22	2.492 (10)
P—PB2	3.546 (17)	O23—O22	4.160 (18)
P—PB2	3.180 (18)	O23—O22	2.831 (16)
P—PB2	4.207 (15)	O23—O22	3.251 (19)
P—PB2	4.380 (14)	O23—O23	4.425 (18)
P—PB2	4.166 (13)	O23—O23	4.425 (18)
P—P^ii	4.264 (15)	O23—O23	4.25 (3)
P—P	4.241 (17)	O23—O1	2.480 (9)
P—P	4.124 (17)	O23—O1	3.48 (2)
P—P	3.917 (8)	O23—O1	3.03 (2)
P—O21	1.543 (8)	O1—PB1	3.21 (2)
P—O21^iii	4.227 (10)	O1—PB1	3.11 (2)
P—O21^ii	4.408 (17)	O1—PB1	3.169 (18)
P—O21	4.14 (2)	O1—PB2	2.353 (8)
P—O21	4.418 (12)	O1—PB2^ii	4.00 (2)
P—O21	3.692 (18)	O1—PB2	4.322 (16)
P—O22^iv	4.465 (11)	O1—PB2	3.937 (18)
P—O22	1.522 (9)	O1—P	1.508 (6)
P—O22^ii	4.309 (17)	O1—P^ii	3.42 (2)
P—O22	4.346 (19)	O1—P	3.53 (2)
P—O22	4.236 (11)	O1—P	3.28 (2)
P—O22	3.622 (16)	O1—O21	2.491 (9)
P—O23	1.529 (9)	O1—O21^ii	3.426 (16)
P—O23	4.379 (18)	O1—O21	3.18 (2)
P—O23	4.120 (18)	O1—O22	2.474 (9)
P—O23	4.422 (17)	O1—O22^ii	3.201 (17)
P—O23	4.166 (16)	O1—O22	3.33 (2)
P—O23	3.787 (16)	O1—O23	2.480 (9)
P—O1	1.508 (6)	O1—O23	3.48 (2)
P—O1^ii	3.42 (2)	O1—O23	3.03 (2)
P—O1	3.53 (2)	O1—O1^ii	3.12 (4)
P—O1	3.28 (2)	O1—O1	3.38 (3)
O21—PB1	2.55 (2)	O1—O1	3.01 (3)
O21—PB1	4.321 (14)
O21—P—O22	109.47 (14)	O22—P—O23	109.45 (12)
O21—P—O23	109.46 (12)	O22—P—O1	109.47 (13)
O21—P—O1	109.48 (13)	O23—P—O1	109.50 (13)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(S2P16_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5551 (8) Å	Particle morphology: Component of pressure cell, not sample
V = 44.93 (3) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.083	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 86.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 110.5 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 228.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.064	48 parameters
Rexp = 0.065	10 restraints
R(F^2) = 0.18021	(Δ/σ)max = 0.03
χ^2 = 1.000	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 8.256520E-02 2: 6.523940E-03 3: 2.208510E-02 4: 2.331650E-04 5: -5.602230E-03 6: -6.446600E-03 7: -5.068810E-03 8: -6.062250E-03 9: 3.249320E-0310: -7.517300E-0311: 1.452010E-0312: -2.585640E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.88185 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.230 (5)	O21—PB2^x	2.99 (2)
PB1—PB2^i	4.230 (5)	O21—PB2^xi	2.80 (2)
PB1—PB2^ii	3.90 (2)	O21—PB2^xii	4.49 (2)
PB1—PB2^iii	4.08 (2)	O21—PB2^viii	2.890 (18)
PB1—PB2^iv	3.90 (2)	O21—PB2^xiii	4.470 (19)
PB1—PB2^v	4.08 (2)	O21—P^xvii	4.227 (10)
PB1—PB2^vi	4.062 (14)	O21—P	1.543 (8)
PB1—PB2^vii	4.062 (14)	O21—P^x	4.408 (17)
PB1—P^ii	3.485 (19)	O21—P^xi	4.14 (2)
PB1—P^iii	3.48 (2)	O21—P^xix	4.418 (12)
PB1—P^iv	3.485 (19)	O21—P^xiv	3.692 (18)
PB1—P^v	3.48 (2)	O21—O21^x	4.27 (3)
PB1—P^vi	3.400 (9)	O21—O21^xxi	4.29 (3)
PB1—P^vii	3.400 (9)	O21—O21^xiv	4.08 (3)
PB1—O21^iii	2.55 (2)	O21—O22^xvii	3.020 (10)
PB1—O21^v	2.55 (2)	O21—O22	2.503 (9)
PB1—O21^vi	4.321 (14)	O21—O22^xxii	4.437 (16)
PB1—O21^vii	4.321 (14)	O21—O22^xiv	3.137 (18)
PB1—O22^ii	2.68 (2)	O21—O23	2.508 (9)
PB1—O22^iii	4.44 (2)	O21—O23^xi	4.097 (18)
PB1—O22^iv	2.68 (2)	O21—O23^xix	3.120 (18)
PB1—O22^v	4.44 (2)	O21—O23^xiv	3.325 (19)
PB1—O23^ii	4.455 (18)	O21—O1	2.491 (9)
PB1—O23^iv	4.455 (18)	O21—O1^x	3.426 (16)
PB1—O23^vi	2.482 (14)	O21—O1^xi	3.18 (2)
PB1—O23^vii	2.482 (14)	O22—PB1^viii	4.44 (2)
PB1—O1^ii	3.11 (2)	O22—PB1^ix	2.68 (2)
PB1—O1^iii	3.21 (2)	O22—PB2^x	2.57 (2)
PB1—O1^iv	3.11 (2)	O22—PB2^xii	2.82 (3)
PB1—O1^v	3.21 (2)	O22—PB2^viii	4.469 (18)
PB1—O1^vi	3.169 (18)	O22—PB2^ix	2.970 (15)
PB1—O1^vii	3.169 (18)	O22—P	1.522 (9)
PB2—PB1	4.230 (5)	O22—P^xv	4.465 (11)
PB2—PB1^viii	4.08 (2)	O22—P^x	4.309 (17)
PB2—PB1^ix	3.90 (2)	O22—P^xii	4.346 (19)
PB2—PB1^vi	4.062 (14)	O22—P^xx	4.236 (11)
PB2—PB2^iv	3.569 (14)	O22—P^xiv	3.622 (16)
PB2—PB2^v	3.569 (14)	O22—O21	2.503 (9)
PB2—PB2^vi	3.74 (3)	O22—O21^xv	3.020 (10)
PB2—P	3.861 (7)	O22—O21^xxiii	4.437 (16)
PB2—P^x	3.30 (2)	O22—O21^xiv	3.137 (18)
PB2—P^xi	3.546 (17)	O22—O22^x	4.28 (2)
PB2—P^xii	3.180 (18)	O22—O22^xiv	3.94 (3)
PB2—P^ii	4.380 (14)	O22—O22^xxiv	4.42 (3)
PB2—P^iii	4.207 (15)	O22—O23	2.492 (10)
PB2—P^vii	4.166 (13)	O22—O23^xii	4.160 (18)
PB2—O21^x	2.99 (2)	O22—O23^xx	2.831 (16)
PB2—O21^xi	2.80 (2)	O22—O23^xiv	3.251 (19)
PB2—O21^xii	4.49 (2)	O22—O1	2.474 (9)
PB2—O21^iii	2.890 (18)	O22—O1^x	3.201 (17)
PB2—O21^vii	4.470 (19)	O22—O1^xii	3.33 (2)
PB2—O22^x	2.57 (2)	O23—PB1^ix	4.455 (18)
PB2—O22^xii	2.82 (3)	O23—PB1^vi	2.482 (14)
PB2—O22^ii	2.970 (15)	O23—PB2^xi	3.151 (18)
PB2—O22^iii	4.469 (18)	O23—PB2^xii	2.498 (18)
PB2—O23^xi	3.151 (18)	O23—PB2^xiii	2.881 (15)
PB2—O23^xii	2.498 (18)	O23—P	1.529 (9)
PB2—O23^vii	2.881 (15)	O23—P^xi	4.379 (18)
PB2—O1	2.353 (8)	O23—P^xii	4.120 (18)
PB2—O1^x	4.00 (2)	O23—P^xvi	4.422 (17)
PB2—O1^xi	4.322 (16)	O23—P^xviii	4.166 (16)
PB2—O1^xii	3.937 (18)	O23—P^xiv	3.787 (16)
P—PB1^viii	3.48 (2)	O23—O21	2.508 (9)
P—PB1^ix	3.485 (19)	O23—O21^xi	4.097 (18)
P—PB1^vi	3.400 (9)	O23—O21^xvi	3.120 (18)
P—PB2	3.861 (7)	O23—O21^xiv	3.325 (19)
P—PB2^x	3.30 (2)	O23—O22	2.492 (10)
P—PB2^xi	3.546 (17)	O23—O22^xii	4.160 (18)
P—PB2^xii	3.180 (18)	O23—O22^xviii	2.831 (16)
P—PB2^viii	4.207 (15)	O23—O22^xiv	3.251 (19)
P—PB2^ix	4.380 (14)	O23—O23^xxv	4.425 (18)
P—PB2^xiii	4.166 (13)	O23—O23^xxvi	4.425 (18)
P—P^x	4.264 (15)	O23—O23^xiv	4.25 (3)
P—P^xi	4.241 (17)	O23—O1	2.480 (9)
P—P^xii	4.124 (17)	O23—O1^xi	3.48 (2)
P—P^xiv	3.917 (8)	O23—O1^xii	3.03 (2)
P—O21	1.543 (8)	O1—PB1^viii	3.21 (2)
P—O21^xv	4.227 (10)	O1—PB1^ix	3.11 (2)
P—O21^x	4.408 (17)	O1—PB1^vi	3.169 (18)
P—O21^xi	4.14 (2)	O1—PB2	2.353 (8)
P—O21^xvi	4.418 (12)	O1—PB2^x	4.00 (2)
P—O21^xiv	3.692 (18)	O1—PB2^xi	4.322 (16)
P—O22^xvii	4.465 (11)	O1—PB2^xii	3.937 (18)
P—O22	1.522 (9)	O1—P	1.508 (6)
P—O22^x	4.309 (17)	O1—P^x	3.42 (2)
P—O22^xii	4.346 (19)	O1—P^xi	3.53 (2)
P—O22^xviii	4.236 (11)	O1—P^xii	3.28 (2)
P—O22^xiv	3.622 (16)	O1—O21	2.491 (9)
P—O23	1.529 (9)	O1—O21^x	3.426 (16)
P—O23^xi	4.379 (18)	O1—O21^xi	3.18 (2)
P—O23^xii	4.120 (18)	O1—O22	2.474 (9)
P—O23^xix	4.422 (17)	O1—O22^x	3.201 (17)
P—O23^xx	4.166 (16)	O1—O22^xii	3.33 (2)
P—O23^xiv	3.787 (16)	O1—O23	2.480 (9)
P—O1	1.508 (6)	O1—O23^xi	3.48 (2)
P—O1^x	3.42 (2)	O1—O23^xii	3.03 (2)
P—O1^xi	3.53 (2)	O1—O1^x	3.12 (4)
P—O1^xii	3.28 (2)	O1—O1^xi	3.38 (3)
O21—PB1^viii	2.55 (2)	O1—O1^xii	3.01 (3)
O21—PB1^vi	4.321 (14)
O21—P—O22	109.47 (14)	O22—P—O23	109.45 (12)
O21—P—O23	109.46 (12)	O22—P—O1	109.47 (13)
O21—P—O1	109.48 (13)	O23—P—O1	109.50 (13)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) x, y+1, z; (xvi) −z, −x, −y+1; (xvii) x, y−1, z; (xviii) −z, −x+1, −y+1; (xix) −z, −x, −y; (xx) −z, −x+1, −y; (xxi) −x+1, −y−1/2, −z+3/2; (xxii) z+1, x−1/2, y+1/2; (xxiii) z+1, x+1/2, y+1/2; (xxiv) −x+1, −y+3/2, −z+3/2; (xxv) z+1, x−1/2, y+3/2; (xxvi) z+1, x+1/2, y+3/2.

(S2P18_phase_1)

Crystal data

O8P2Pb3	V = 692.82 (9) Å^3
Mr = 811.74	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7371 (11) Å	T = 298 K
b = 5.4905 (6) Å	Particle morphology: plate
c = 9.4299 (9) Å	irregular, 6 × 6 mm
β = 103.068 (10)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.097	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 0.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 141.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 118.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.082	48 parameters
Rexp = 0.074	10 restraints
R(F^2) = 0.25751	(Δ/σ)max = 0.06
χ^2 = 1.254	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 7.397510E-02 2: 1.978690E-02 3: 1.988520E-02 4: 1.423360E-02 5: -3.490920E-03 6: 4.332530E-03 7: -2.682000E-03 8: 1.848130E-03 9: 3.043180E-0310: -1.316140E-0411: -1.344790E-0312: 1.234110E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.87963 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
PB1	0.0	0.254 (5)	0.25	0.025 (3)*
PB2	0.3156 (4)	0.280 (3)	0.3482 (19)	0.025 (3)*
P	0.6045 (4)	0.259 (2)	0.4563 (11)	0.010 (3)*
O21	0.6402 (11)	0.017 (3)	0.4052 (18)	0.0111 (19)*
O22	0.6497 (10)	0.469 (3)	0.3875 (17)	0.0111 (19)*
O23	0.6374 (10)	0.277 (3)	0.6213 (13)	0.0111 (19)*
O1	0.4916 (5)	0.273 (3)	0.411 (2)	0.0111 (19)*

Geometric parameters (Å, º)

PB1—PB2	4.226 (6)	O21—PB2^xi	2.79 (3)
PB1—PB2^i	4.226 (6)	O21—PB2^xii	4.48 (2)
PB1—PB2^ii	3.89 (3)	O21—PB2^viii	2.89 (2)
PB1—PB2^iii	4.08 (3)	O21—PB2^xiii	4.47 (2)
PB1—PB2^iv	3.89 (3)	O21—P^xvii	4.228 (12)
PB1—PB2^v	4.08 (3)	O21—P	1.534 (10)
PB1—PB2^vi	4.058 (15)	O21—P^x	4.42 (2)
PB1—PB2^vii	4.058 (15)	O21—P^xi	4.16 (2)
PB1—P^ii	3.46 (2)	O21—P^xix	4.418 (15)
PB1—P^iii	3.50 (2)	O21—P^xiv	3.67 (2)
PB1—P^iv	3.46 (2)	O21—O21^x	4.28 (3)
PB1—P^v	3.50 (2)	O21—O21^xxi	4.29 (3)
PB1—P^vi	3.396 (10)	O21—O21^xiv	4.05 (3)
PB1—P^vii	3.396 (10)	O21—O22^xvii	3.015 (11)
PB1—O21^iii	2.58 (2)	O21—O22	2.495 (11)
PB1—O21^v	2.58 (2)	O21—O22^xxii	4.429 (17)
PB1—O21^vi	4.324 (16)	O21—O22^xiv	3.10 (2)
PB1—O21^vii	4.324 (16)	O21—O23	2.495 (11)
PB1—O22^ii	2.68 (2)	O21—O23^xi	4.09 (2)
PB1—O22^iii	4.48 (3)	O21—O23^xix	3.12 (2)
PB1—O22^iv	2.68 (2)	O21—O23^xiv	3.32 (2)
PB1—O22^v	4.48 (3)	O21—O1	2.489 (10)
PB1—O23^ii	4.44 (2)	O21—O1^x	3.421 (19)
PB1—O23^iv	4.44 (2)	O21—O1^xi	3.20 (3)
PB1—O23^vi	2.469 (15)	O22—PB1^viii	4.48 (3)
PB1—O23^vii	2.469 (15)	O22—PB1^ix	2.68 (2)
PB1—O1^ii	3.07 (3)	O22—PB2^x	2.59 (3)
PB1—O1^iii	3.24 (3)	O22—PB2^xii	2.79 (3)
PB1—O1^iv	3.07 (3)	O22—PB2^viii	4.47 (2)
PB1—O1^v	3.24 (3)	O22—PB2^ix	2.938 (18)
PB1—O1^vi	3.176 (18)	O22—P	1.522 (10)
PB1—O1^vii	3.176 (18)	O22—P^xv	4.450 (13)
PB2—PB1	4.226 (6)	O22—P^x	4.349 (19)
PB2—PB1^viii	4.08 (3)	O22—P^xii	4.35 (2)
PB2—PB1^ix	3.89 (3)	O22—P^xx	4.243 (13)
PB2—PB1^vi	4.058 (15)	O22—P^xiv	3.591 (19)
PB2—PB2^iv	3.564 (15)	O22—O21	2.495 (11)
PB2—PB2^v	3.564 (15)	O22—O21^xv	3.015 (11)
PB2—PB2^vi	3.73 (3)	O22—O21^xxiii	4.429 (17)
PB2—P	3.869 (8)	O22—O21^xiv	3.10 (2)
PB2—P^x	3.30 (2)	O22—O22^x	4.34 (3)
PB2—P^xi	3.53 (2)	O22—O22^xiv	3.90 (3)
PB2—P^xii	3.18 (2)	O22—O22^xxiv	4.35 (3)
PB2—P^ii	4.356 (17)	O22—O23	2.486 (11)
PB2—P^iii	4.207 (18)	O22—O23^xii	4.17 (2)
PB2—P^vii	4.156 (15)	O22—O23^xx	2.844 (19)
PB2—O21^x	2.97 (3)	O22—O23^xiv	3.24 (2)
PB2—O21^xi	2.79 (3)	O22—O1	2.479 (10)
PB2—O21^xii	4.48 (2)	O22—O1^x	3.223 (19)
PB2—O21^iii	2.89 (2)	O22—O1^xii	3.33 (3)
PB2—O21^vii	4.47 (2)	O23—PB1^ix	4.44 (2)
PB2—O22^x	2.59 (3)	O23—PB1^vi	2.469 (15)
PB2—O22^xii	2.79 (3)	O23—PB2^xi	3.13 (2)
PB2—O22^ii	2.938 (18)	O23—PB2^xii	2.52 (2)
PB2—O22^iii	4.47 (2)	O23—PB2^xiii	2.881 (16)
PB2—O23^xi	3.13 (2)	O23—P	1.523 (10)
PB2—O23^xii	2.52 (2)	O23—P^xi	4.37 (2)
PB2—O23^vii	2.881 (16)	O23—P^xii	4.12 (2)
PB2—O1	2.357 (9)	O23—P^xvi	4.41 (2)
PB2—O1^x	3.99 (2)	O23—P^xviii	4.162 (19)
PB2—O1^xi	4.321 (18)	O23—P^xiv	3.785 (17)
PB2—O1^xii	3.934 (19)	O23—O21	2.495 (11)
P—PB1^viii	3.50 (2)	O23—O21^xi	4.09 (2)
P—PB1^ix	3.46 (2)	O23—O21^xvi	3.12 (2)
P—PB1^vi	3.396 (10)	O23—O21^xiv	3.32 (2)
P—PB2	3.869 (8)	O23—O22	2.486 (11)
P—PB2^x	3.30 (2)	O23—O22^xii	4.17 (2)
P—PB2^xi	3.53 (2)	O23—O22^xviii	2.844 (19)
P—PB2^xii	3.18 (2)	O23—O22^xiv	3.24 (2)
P—PB2^viii	4.207 (18)	O23—O23^xxv	4.427 (19)
P—PB2^ix	4.356 (17)	O23—O23^xxvi	4.427 (19)
P—PB2^xiii	4.156 (15)	O23—O23^xiv	4.25 (3)
P—P^x	4.281 (16)	O23—O1	2.480 (10)
P—P^xi	4.254 (19)	O23—O1^xi	3.48 (2)
P—P^xii	4.121 (19)	O23—O1^xii	3.02 (2)
P—P^xiv	3.897 (10)	O23—O1^xviii	4.48 (2)
P—O21	1.534 (10)	O1—PB1^viii	3.24 (3)
P—O21^xv	4.228 (12)	O1—PB1^ix	3.07 (3)
P—O21^x	4.42 (2)	O1—PB1^vi	3.176 (18)
P—O21^xi	4.16 (2)	O1—PB2	2.357 (9)
P—O21^xvi	4.418 (15)	O1—PB2^x	3.99 (2)
P—O21^xiv	3.67 (2)	O1—PB2^xi	4.321 (18)
P—O22^xvii	4.450 (13)	O1—PB2^xii	3.934 (19)
P—O22	1.522 (10)	O1—P	1.514 (8)
P—O22^x	4.349 (19)	O1—P^x	3.42 (2)
P—O22^xii	4.35 (2)	O1—P^xi	3.55 (2)
P—O22^xviii	4.243 (13)	O1—P^xii	3.27 (3)
P—O22^xiv	3.591 (19)	O1—O21	2.489 (10)
P—O23	1.523 (10)	O1—O21^x	3.421 (19)
P—O23^xi	4.37 (2)	O1—O21^xi	3.20 (3)
P—O23^xii	4.12 (2)	O1—O22	2.479 (10)
P—O23^xix	4.41 (2)	O1—O22^x	3.223 (19)
P—O23^xx	4.162 (19)	O1—O22^xii	3.33 (3)
P—O23^xiv	3.785 (17)	O1—O23	2.480 (10)
P—O1	1.514 (8)	O1—O23^xi	3.48 (2)
P—O1^x	3.42 (2)	O1—O23^xii	3.02 (2)
P—O1^xi	3.55 (2)	O1—O23^xx	4.48 (2)
P—O1^xii	3.27 (3)	O1—O1^x	3.10 (4)
O21—PB1^viii	2.58 (2)	O1—O1^xi	3.42 (3)
O21—PB1^vi	4.324 (16)	O1—O1^xii	2.99 (4)
O21—PB2^x	2.97 (3)
O21—P—O22	109.47 (15)	O22—P—O23	109.45 (13)
O21—P—O23	109.45 (13)	O22—P—O1	109.48 (14)
O21—P—O1	109.48 (15)	O23—P—O1	109.50 (15)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, y−1, z; (xviii) x, −y+1, z+3/2; (xix) x, −y, z+1/2; (xx) x, −y+1, z+1/2; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2; (xxiv) −x+3/2, −y+3/2, −z+1; (xxv) −x+3/2, y−1/2, −z+3/2; (xxvi) −x+3/2, y+1/2, −z+3/2.

(S2P18_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8994 (12) Å	T = 298 K
c = 2.8273 (18) Å	Particle morphology: Pressure cell anvil material
V = 20.58 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.097	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 0.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 141.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 118.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.082	48 parameters
Rexp = 0.074	10 restraints
R(F^2) = 0.25751	(Δ/σ)max = 0.06
χ^2 = 1.254	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 7.397510E-02 2: 1.978690E-02 3: 1.988520E-02 4: 1.423360E-02 5: -3.490920E-03 6: 4.332530E-03 7: -2.682000E-03 8: 1.848130E-03 9: 3.043180E-0310: -1.316140E-0411: -1.344790E-0312: 1.234110E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.87963 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.226 (6)	O21—PB2	2.79 (3)
PB1—PB2^i	4.226 (6)	O21—PB2	4.48 (2)
PB1—PB2	3.89 (3)	O21—PB2	2.89 (2)
PB1—PB2	4.08 (3)	O21—PB2	4.47 (2)
PB1—PB2	3.89 (3)	O21—P^iv	4.228 (12)
PB1—PB2	4.08 (3)	O21—P	1.534 (10)
PB1—PB2	4.058 (15)	O21—P^ii	4.42 (2)
PB1—PB2	4.058 (15)	O21—P	4.16 (2)
PB1—P	3.46 (2)	O21—P	4.418 (15)
PB1—P	3.50 (2)	O21—P	3.67 (2)
PB1—P	3.46 (2)	O21—O21^ii	4.28 (3)
PB1—P	3.50 (2)	O21—O21	4.29 (3)
PB1—P	3.396 (10)	O21—O21	4.05 (3)
PB1—P	3.396 (10)	O21—O22^iv	3.015 (11)
PB1—O21	2.58 (2)	O21—O22	2.495 (11)
PB1—O21	2.58 (2)	O21—O22	4.429 (17)
PB1—O21	4.324 (16)	O21—O22	3.10 (2)
PB1—O21	4.324 (16)	O21—O23	2.495 (11)
PB1—O22	2.68 (2)	O21—O23	4.09 (2)
PB1—O22	4.48 (3)	O21—O23	3.12 (2)
PB1—O22	2.68 (2)	O21—O23	3.32 (2)
PB1—O22	4.48 (3)	O21—O1	2.489 (10)
PB1—O23	4.44 (2)	O21—O1^ii	3.421 (19)
PB1—O23	4.44 (2)	O21—O1	3.20 (3)
PB1—O23	2.469 (15)	O22—PB1	4.48 (3)
PB1—O23	2.469 (15)	O22—PB1	2.68 (2)
PB1—O1	3.07 (3)	O22—PB2^ii	2.59 (3)
PB1—O1	3.24 (3)	O22—PB2	2.79 (3)
PB1—O1	3.07 (3)	O22—PB2	4.47 (2)
PB1—O1	3.24 (3)	O22—PB2	2.938 (18)
PB1—O1	3.176 (18)	O22—P	1.522 (10)
PB1—O1	3.176 (18)	O22—P^iii	4.450 (13)
PB2—PB1	4.226 (6)	O22—P^ii	4.349 (19)
PB2—PB1	4.08 (3)	O22—P	4.35 (2)
PB2—PB1	3.89 (3)	O22—P	4.243 (13)
PB2—PB1	4.058 (15)	O22—P	3.591 (19)
PB2—PB2	3.564 (15)	O22—O21	2.495 (11)
PB2—PB2	3.564 (15)	O22—O21^iii	3.015 (11)
PB2—PB2	3.73 (3)	O22—O21	4.429 (17)
PB2—P	3.869 (8)	O22—O21	3.10 (2)
PB2—P^ii	3.30 (2)	O22—O22^ii	4.34 (3)
PB2—P	3.53 (2)	O22—O22	3.90 (3)
PB2—P	3.18 (2)	O22—O22	4.35 (3)
PB2—P	4.356 (17)	O22—O23	2.486 (11)
PB2—P	4.207 (18)	O22—O23	4.17 (2)
PB2—P	4.156 (15)	O22—O23	2.844 (19)
PB2—O21^ii	2.97 (3)	O22—O23	3.24 (2)
PB2—O21	2.79 (3)	O22—O1	2.479 (10)
PB2—O21	4.48 (2)	O22—O1^ii	3.223 (19)
PB2—O21	2.89 (2)	O22—O1	3.33 (3)
PB2—O21	4.47 (2)	O23—PB1	4.44 (2)
PB2—O22^ii	2.59 (3)	O23—PB1	2.469 (15)
PB2—O22	2.79 (3)	O23—PB2	3.13 (2)
PB2—O22	2.938 (18)	O23—PB2	2.52 (2)
PB2—O22	4.47 (2)	O23—PB2	2.881 (16)
PB2—O23	3.13 (2)	O23—P	1.523 (10)
PB2—O23	2.52 (2)	O23—P	4.37 (2)
PB2—O23	2.881 (16)	O23—P	4.12 (2)
PB2—O1	2.357 (9)	O23—P	4.41 (2)
PB2—O1^ii	3.99 (2)	O23—P	4.162 (19)
PB2—O1	4.321 (18)	O23—P	3.785 (17)
PB2—O1	3.934 (19)	O23—O21	2.495 (11)
P—PB1	3.50 (2)	O23—O21	4.09 (2)
P—PB1	3.46 (2)	O23—O21	3.12 (2)
P—PB1	3.396 (10)	O23—O21	3.32 (2)
P—PB2	3.869 (8)	O23—O22	2.486 (11)
P—PB2^ii	3.30 (2)	O23—O22	4.17 (2)
P—PB2	3.53 (2)	O23—O22	2.844 (19)
P—PB2	3.18 (2)	O23—O22	3.24 (2)
P—PB2	4.207 (18)	O23—O23	4.427 (19)
P—PB2	4.356 (17)	O23—O23	4.427 (19)
P—PB2	4.156 (15)	O23—O23	4.25 (3)
P—P^ii	4.281 (16)	O23—O1	2.480 (10)
P—P	4.254 (19)	O23—O1	3.48 (2)
P—P	4.121 (19)	O23—O1	3.02 (2)
P—P	3.897 (10)	O23—O1	4.48 (2)
P—O21	1.534 (10)	O1—PB1	3.24 (3)
P—O21^iii	4.228 (12)	O1—PB1	3.07 (3)
P—O21^ii	4.42 (2)	O1—PB1	3.176 (18)
P—O21	4.16 (2)	O1—PB2	2.357 (9)
P—O21	4.418 (15)	O1—PB2^ii	3.99 (2)
P—O21	3.67 (2)	O1—PB2	4.321 (18)
P—O22^iv	4.450 (13)	O1—PB2	3.934 (19)
P—O22	1.522 (10)	O1—P	1.514 (8)
P—O22^ii	4.349 (19)	O1—P^ii	3.42 (2)
P—O22	4.35 (2)	O1—P	3.55 (2)
P—O22	4.243 (13)	O1—P	3.27 (3)
P—O22	3.591 (19)	O1—O21	2.489 (10)
P—O23	1.523 (10)	O1—O21^ii	3.421 (19)
P—O23	4.37 (2)	O1—O21	3.20 (3)
P—O23	4.12 (2)	O1—O22	2.479 (10)
P—O23	4.41 (2)	O1—O22^ii	3.223 (19)
P—O23	4.162 (19)	O1—O22	3.33 (3)
P—O23	3.785 (17)	O1—O23	2.480 (10)
P—O1	1.514 (8)	O1—O23	3.48 (2)
P—O1^ii	3.42 (2)	O1—O23	3.02 (2)
P—O1	3.55 (2)	O1—O23	4.48 (2)
P—O1	3.27 (3)	O1—O1^ii	3.10 (4)
O21—PB1	2.58 (2)	O1—O1	3.42 (3)
O21—PB1	4.324 (16)	O1—O1	2.99 (4)
O21—PB2^ii	2.97 (3)
O21—P—O22	109.47 (15)	O22—P—O23	109.45 (13)
O21—P—O23	109.45 (13)	O22—P—O1	109.48 (14)
O21—P—O1	109.48 (15)	O23—P—O1	109.50 (15)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(S2P18_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5554 (9) Å	Particle morphology: Component of pressure cell, not sample
V = 44.94 (4) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.853 < d <3.015 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.097	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 0.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.21 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 141.3 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 118.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.082	48 parameters
Rexp = 0.074	10 restraints
R(F^2) = 0.25751	(Δ/σ)max = 0.06
χ^2 = 1.254	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 7.397510E-02 2: 1.978690E-02 3: 1.988520E-02 4: 1.423360E-02 5: -3.490920E-03 6: 4.332530E-03 7: -2.682000E-03 8: 1.848130E-03 9: 3.043180E-0310: -1.316140E-0411: -1.344790E-0312: 1.234110E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.87963 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.226 (6)	O21—PB2^xi	2.79 (3)
PB1—PB2^i	4.226 (6)	O21—PB2^xii	4.48 (2)
PB1—PB2^ii	3.89 (3)	O21—PB2^viii	2.89 (2)
PB1—PB2^iii	4.08 (3)	O21—PB2^xiii	4.47 (2)
PB1—PB2^iv	3.89 (3)	O21—P^xvii	4.228 (12)
PB1—PB2^v	4.08 (3)	O21—P	1.534 (10)
PB1—PB2^vi	4.058 (15)	O21—P^x	4.42 (2)
PB1—PB2^vii	4.058 (15)	O21—P^xi	4.16 (2)
PB1—P^ii	3.46 (2)	O21—P^xix	4.418 (15)
PB1—P^iii	3.50 (2)	O21—P^xiv	3.67 (2)
PB1—P^iv	3.46 (2)	O21—O21^x	4.28 (3)
PB1—P^v	3.50 (2)	O21—O21^xxi	4.29 (3)
PB1—P^vi	3.396 (10)	O21—O21^xiv	4.05 (3)
PB1—P^vii	3.396 (10)	O21—O22^xvii	3.015 (11)
PB1—O21^iii	2.58 (2)	O21—O22	2.495 (11)
PB1—O21^v	2.58 (2)	O21—O22^xxii	4.429 (17)
PB1—O21^vi	4.324 (16)	O21—O22^xiv	3.10 (2)
PB1—O21^vii	4.324 (16)	O21—O23	2.495 (11)
PB1—O22^ii	2.68 (2)	O21—O23^xi	4.09 (2)
PB1—O22^iii	4.48 (3)	O21—O23^xix	3.12 (2)
PB1—O22^iv	2.68 (2)	O21—O23^xiv	3.32 (2)
PB1—O22^v	4.48 (3)	O21—O1	2.489 (10)
PB1—O23^ii	4.44 (2)	O21—O1^x	3.421 (19)
PB1—O23^iv	4.44 (2)	O21—O1^xi	3.20 (3)
PB1—O23^vi	2.469 (15)	O22—PB1^viii	4.48 (3)
PB1—O23^vii	2.469 (15)	O22—PB1^ix	2.68 (2)
PB1—O1^ii	3.07 (3)	O22—PB2^x	2.59 (3)
PB1—O1^iii	3.24 (3)	O22—PB2^xii	2.79 (3)
PB1—O1^iv	3.07 (3)	O22—PB2^viii	4.47 (2)
PB1—O1^v	3.24 (3)	O22—PB2^ix	2.938 (18)
PB1—O1^vi	3.176 (18)	O22—P	1.522 (10)
PB1—O1^vii	3.176 (18)	O22—P^xv	4.450 (13)
PB2—PB1	4.226 (6)	O22—P^x	4.349 (19)
PB2—PB1^viii	4.08 (3)	O22—P^xii	4.35 (2)
PB2—PB1^ix	3.89 (3)	O22—P^xx	4.243 (13)
PB2—PB1^vi	4.058 (15)	O22—P^xiv	3.591 (19)
PB2—PB2^iv	3.564 (15)	O22—O21	2.495 (11)
PB2—PB2^v	3.564 (15)	O22—O21^xv	3.015 (11)
PB2—PB2^vi	3.73 (3)	O22—O21^xxiii	4.429 (17)
PB2—P	3.869 (8)	O22—O21^xiv	3.10 (2)
PB2—P^x	3.30 (2)	O22—O22^x	4.34 (3)
PB2—P^xi	3.53 (2)	O22—O22^xiv	3.90 (3)
PB2—P^xii	3.18 (2)	O22—O22^xxiv	4.35 (3)
PB2—P^ii	4.356 (17)	O22—O23	2.486 (11)
PB2—P^iii	4.207 (18)	O22—O23^xii	4.17 (2)
PB2—P^vii	4.156 (15)	O22—O23^xx	2.844 (19)
PB2—O21^x	2.97 (3)	O22—O23^xiv	3.24 (2)
PB2—O21^xi	2.79 (3)	O22—O1	2.479 (10)
PB2—O21^xii	4.48 (2)	O22—O1^x	3.223 (19)
PB2—O21^iii	2.89 (2)	O22—O1^xii	3.33 (3)
PB2—O21^vii	4.47 (2)	O23—PB1^ix	4.44 (2)
PB2—O22^x	2.59 (3)	O23—PB1^vi	2.469 (15)
PB2—O22^xii	2.79 (3)	O23—PB2^xi	3.13 (2)
PB2—O22^ii	2.938 (18)	O23—PB2^xii	2.52 (2)
PB2—O22^iii	4.47 (2)	O23—PB2^xiii	2.881 (16)
PB2—O23^xi	3.13 (2)	O23—P	1.523 (10)
PB2—O23^xii	2.52 (2)	O23—P^xi	4.37 (2)
PB2—O23^vii	2.881 (16)	O23—P^xii	4.12 (2)
PB2—O1	2.357 (9)	O23—P^xvi	4.41 (2)
PB2—O1^x	3.99 (2)	O23—P^xviii	4.162 (19)
PB2—O1^xi	4.321 (18)	O23—P^xiv	3.785 (17)
PB2—O1^xii	3.934 (19)	O23—O21	2.495 (11)
P—PB1^viii	3.50 (2)	O23—O21^xi	4.09 (2)
P—PB1^ix	3.46 (2)	O23—O21^xvi	3.12 (2)
P—PB1^vi	3.396 (10)	O23—O21^xiv	3.32 (2)
P—PB2	3.869 (8)	O23—O22	2.486 (11)
P—PB2^x	3.30 (2)	O23—O22^xii	4.17 (2)
P—PB2^xi	3.53 (2)	O23—O22^xviii	2.844 (19)
P—PB2^xii	3.18 (2)	O23—O22^xiv	3.24 (2)
P—PB2^viii	4.207 (18)	O23—O23^xxv	4.427 (19)
P—PB2^ix	4.356 (17)	O23—O23^xxvi	4.427 (19)
P—PB2^xiii	4.156 (15)	O23—O23^xiv	4.25 (3)
P—P^x	4.281 (16)	O23—O1	2.480 (10)
P—P^xi	4.254 (19)	O23—O1^xi	3.48 (2)
P—P^xii	4.121 (19)	O23—O1^xii	3.02 (2)
P—P^xiv	3.897 (10)	O23—O1^xviii	4.48 (2)
P—O21	1.534 (10)	O1—PB1^viii	3.24 (3)
P—O21^xv	4.228 (12)	O1—PB1^ix	3.07 (3)
P—O21^x	4.42 (2)	O1—PB1^vi	3.176 (18)
P—O21^xi	4.16 (2)	O1—PB2	2.357 (9)
P—O21^xvi	4.418 (15)	O1—PB2^x	3.99 (2)
P—O21^xiv	3.67 (2)	O1—PB2^xi	4.321 (18)
P—O22^xvii	4.450 (13)	O1—PB2^xii	3.934 (19)
P—O22	1.522 (10)	O1—P	1.514 (8)
P—O22^x	4.349 (19)	O1—P^x	3.42 (2)
P—O22^xii	4.35 (2)	O1—P^xi	3.55 (2)
P—O22^xviii	4.243 (13)	O1—P^xii	3.27 (3)
P—O22^xiv	3.591 (19)	O1—O21	2.489 (10)
P—O23	1.523 (10)	O1—O21^x	3.421 (19)
P—O23^xi	4.37 (2)	O1—O21^xi	3.20 (3)
P—O23^xii	4.12 (2)	O1—O22	2.479 (10)
P—O23^xix	4.41 (2)	O1—O22^x	3.223 (19)
P—O23^xx	4.162 (19)	O1—O22^xii	3.33 (3)
P—O23^xiv	3.785 (17)	O1—O23	2.480 (10)
P—O1	1.514 (8)	O1—O23^xi	3.48 (2)
P—O1^x	3.42 (2)	O1—O23^xii	3.02 (2)
P—O1^xi	3.55 (2)	O1—O23^xx	4.48 (2)
P—O1^xii	3.27 (3)	O1—O1^x	3.10 (4)
O21—PB1^viii	2.58 (2)	O1—O1^xi	3.42 (3)
O21—PB1^vi	4.324 (16)	O1—O1^xii	2.99 (4)
O21—PB2^x	2.97 (3)
O21—P—O22	109.47 (15)	O22—P—O23	109.45 (13)
O21—P—O23	109.45 (13)	O22—P—O1	109.48 (14)
O21—P—O1	109.48 (15)	O23—P—O1	109.50 (15)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) x, y+1, z; (xvi) −z, −x, −y+1; (xvii) x, y−1, z; (xviii) −z, −x+1, −y+1; (xix) −z, −x, −y; (xx) −z, −x+1, −y; (xxi) −x+1, −y−1/2, −z+3/2; (xxii) z+1, x−1/2, y+1/2; (xxiii) z+1, x+1/2, y+1/2; (xxiv) −x+1, −y+3/2, −z+3/2; (xxv) z+1, x−1/2, y+3/2; (xxvi) z+1, x+1/2, y+3/2.

(S2P19D_phase_1)

Crystal data

O8.00P2Pb3.00	Z = 3
Mr = 811.74	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.4614 (2) Å	Particle morphology: plate
c = 20.0706 (11) Å	irregular, 6 × 6 mm
V = 518.44 (4) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.883 < d <3.007 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 90.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 9.23 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 128.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 241.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.044	36 parameters
Rexp = 0.039	9 restraints
R(F^2) = 0.18408	(Δ/σ)max = 0.01
χ^2 = 1.277	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.505026 2: -3.751250E-03 3: 0.259623 4: -2.540250E-02 5: 7.578030E-02 6: -4.593390E-02 7: 4.408820E-02 8: -2.570450E-02 9: 4.284580E-0210: -1.657270E-0211: 1.488630E-0212: -5.843410E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89345 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
PB1	0.0	0.0	0.0	0.0186 (11)*
PB2	0.0	0.0472 (16)	0.21026 (15)	0.0186 (11)*	0.16667
P	0.0	0.0	0.4022 (2)	0.0168 (13)*
O1	0.0244 (10)	−0.0244 (10)	0.32743 (19)	0.0091 (8)*	0.3333
O2	−0.1285 (12)	0.1760 (11)	0.42871 (12)	0.0091 (8)*	0.5

Geometric parameters (Å, º)

PB1—PB2	4.228 (3)	P—PB2^lxx	4.081 (7)
PB1—PB2^i	4.228 (3)	P—PB2^lxxi	4.250 (4)
PB1—PB2^ii	4.228 (3)	P—PB2^lxxii	4.081 (7)
PB1—PB2^iii	4.228 (3)	P—PB2^lxxiii	4.081 (7)
PB1—PB2^iv	4.228 (3)	P—PB2^lxxiv	4.250 (4)
PB1—PB2^v	4.228 (3)	P—PB2^lxxv	4.250 (4)
PB1—PB2^vi	4.228 (3)	P—PB2^lxxvi	4.081 (7)
PB1—PB2^vii	4.228 (3)	P—PB2^lxxvii	4.081 (7)
PB1—PB2^viii	4.228 (3)	P—PB2^lxxviii	4.250 (4)
PB1—PB2^ix	4.228 (3)	P—P^lxxix	3.928 (9)
PB1—PB2^x	4.228 (3)	P—P^li	4.192 (6)
PB1—PB2^xi	4.228 (3)	P—P^lii	4.192 (6)
PB1—PB2^xii	4.014 (2)	P—P^liii	4.192 (6)
PB1—PB2^xiii	3.834 (6)	P—O1	1.518 (5)
PB1—PB2^xiv	4.186 (6)	P—O1^i	1.518 (5)
PB1—PB2^xv	4.186 (6)	P—O1^ii	1.518 (5)
PB1—PB2^xvi	4.014 (2)	P—O1^li	3.510 (6)
PB1—PB2^xvii	3.834 (6)	P—O1^lii	3.184 (9)
PB1—PB2^xviii	3.834 (6)	P—O1^liii	3.510 (6)
PB1—PB2^xix	4.186 (6)	P—O1^liv	3.510 (6)
PB1—PB2^xx	4.014 (2)	P—O1^lv	3.510 (6)
PB1—PB2^xxi	3.834 (6)	P—O1^lvi	3.184 (9)
PB1—PB2^xxii	4.014 (2)	P—O1^lvii	3.184 (9)
PB1—PB2^xxiii	4.186 (6)	P—O1^lviii	3.510 (6)
PB1—PB2^xxiv	4.186 (6)	P—O1^lix	3.510 (6)
PB1—PB2^xxv	3.834 (6)	P—O2^lxxx	4.227 (4)
PB1—PB2^xxvi	4.014 (2)	P—O2	1.541 (3)
PB1—PB2^xxvii	4.014 (2)	P—O2^lxxxi	4.392 (5)
PB1—PB2^xxviii	4.186 (6)	P—O2^i	1.541 (3)
PB1—PB2^xxix	3.834 (6)	P—O2^lxxxii	4.392 (5)
PB1—PB2^xxx	4.186 (6)	P—O2^lxxxiii	4.227 (4)
PB1—PB2^xxxi	3.834 (6)	P—O2^lxxxiv	4.392 (5)
PB1—PB2^xxxii	4.014 (2)	P—O2^lxxxv	4.227 (4)
PB1—PB2^xxxiii	3.834 (6)	P—O2^ii	1.541 (3)
PB1—PB2^xxxiv	4.014 (2)	P—O2^lxxxvi	4.227 (4)
PB1—PB2^xxxv	4.186 (6)	P—O2^lxxxvii	4.392 (5)
PB1—PB2^xxxvi	4.014 (2)	P—O2^iii	1.541 (3)
PB1—PB2^xxxvii	4.186 (6)	P—O2^lxxxviii	4.392 (5)
PB1—PB2^xxxviii	3.834 (6)	P—O2^iv	1.541 (3)
PB1—PB2^xxxix	4.186 (6)	P—O2^lxxxix	4.227 (4)
PB1—PB2^xl	4.014 (2)	P—O2^v	1.541 (3)
PB1—PB2^xli	3.834 (6)	P—O2^xc	4.227 (4)
PB1—PB2^xlii	4.014 (2)	P—O2^xci	4.392 (5)
PB1—PB2^xliii	3.834 (6)	P—O2^lxxix	3.690 (5)
PB1—PB2^xliv	4.186 (6)	P—O2^xcii	3.690 (5)
PB1—PB2^xlv	3.834 (6)	P—O2^xciii	3.690 (5)
PB1—PB2^xlvi	4.186 (6)	P—O2^xciv	3.690 (5)
PB1—PB2^xlvii	4.014 (2)	P—O2^xcv	3.690 (5)
PB1—P^xii	3.4424 (19)	P—O2^xcvi	3.690 (5)
PB1—P^xiii	3.4424 (19)	P—O2^li	4.366 (6)
PB1—P^xiv	3.4424 (19)	P—O2^liii	4.201 (6)
PB1—P^xxx	3.4424 (19)	P—O2^liv	4.201 (6)
PB1—P^xxxi	3.4424 (19)	P—O2^lv	4.366 (6)
PB1—P^xxxii	3.4424 (19)	P—O2^lviii	4.201 (6)
PB1—O1^xii	3.047 (4)	P—O2^lix	4.366 (6)
PB1—O1^xiii	3.386 (10)	P—O2^lx	4.366 (6)
PB1—O1^xiv	3.047 (4)	P—O2^lxi	4.201 (6)
PB1—O1^xv	3.047 (4)	P—O2^lxii	4.201 (6)
PB1—O1^xvi	3.047 (4)	P—O2^lxiii	4.366 (6)
PB1—O1^xvii	3.386 (10)	P—O2^lxiv	4.366 (6)
PB1—O1^xviii	3.386 (10)	P—O2^lxv	4.201 (6)
PB1—O1^xix	3.047 (4)	O1—PB1^xlviii	3.047 (4)
PB1—O1^xx	3.047 (4)	O1—PB1^xlix	3.386 (10)
PB1—O1^xxx	3.047 (4)	O1—PB1^l	3.047 (4)
PB1—O1^xxxi	3.386 (10)	O1—PB2	2.399 (6)
PB1—O1^xxxii	3.047 (4)	O1—PB2^i	2.377 (5)
PB1—O1^xxxiii	3.386 (10)	O1—PB2^ii	2.355 (5)
PB1—O1^xxxiv	3.047 (4)	O1—PB2^iii	2.377 (5)
PB1—O1^xxxv	3.047 (4)	O1—PB2^iv	2.399 (6)
PB1—O1^xxxvi	3.047 (4)	O1—PB2^v	2.355 (5)
PB1—O1^xxxvii	3.047 (4)	O1—PB2^li	4.170 (5)
PB1—O1^xxxviii	3.386 (10)	O1—PB2^lii	4.076 (9)
PB1—O2^xiii	2.572 (3)	O1—PB2^liii	3.997 (7)
PB1—O2^xvii	2.572 (3)	O1—PB2^liv	4.010 (7)
PB1—O2^xviii	2.572 (3)	O1—PB2^lv	3.913 (8)
PB1—O2^xxi	2.572 (3)	O1—PB2^lvi	4.347 (8)
PB1—O2^xxv	2.572 (3)	O1—PB2^lvii	4.359 (9)
PB1—O2^xxix	2.572 (3)	O1—PB2^lviii	3.742 (9)
PB1—O2^xxxi	2.572 (3)	O1—PB2^lix	4.195 (6)
PB1—O2^xxxiii	2.572 (3)	O1—PB2^lxvi	4.347 (8)
PB1—O2^xxxviii	2.572 (3)	O1—PB2^lx	3.913 (8)
PB1—O2^xli	2.572 (3)	O1—PB2^lxi	4.010 (7)
PB1—O2^xliii	2.572 (3)	O1—PB2^lxii	3.997 (7)
PB1—O2^xlv	2.572 (3)	O1—PB2^lxvii	4.076 (9)
PB2—PB1	4.228 (3)	O1—PB2^lxiii	4.170 (5)
PB2—PB1^xlviii	4.186 (6)	O1—PB2^lxiv	4.195 (6)
PB2—PB1^xlix	3.834 (6)	O1—PB2^lxv	3.742 (9)
PB2—PB1^l	4.014 (2)	O1—PB2^lxviii	4.359 (9)
PB2—PB2^i	0.447 (15)	O1—P	1.518 (5)
PB2—PB2^ii	0.447 (15)	O1—P^li	3.510 (6)
PB2—PB2^iii	0.258 (9)	O1—P^lii	3.184 (9)
PB2—PB2^iv	0.258 (9)	O1—P^liii	3.510 (6)
PB2—PB2^v	0.516 (17)	O1—O1^i	0.399 (17)
PB2—PB2^xxx	4.011 (14)	O1—O1^ii	0.399 (17)
PB2—PB2^xxxi	3.233 (12)	O1—O1^li	3.415 (12)
PB2—PB2^xxxii	3.643 (4)	O1—O1^lii	2.702 (19)
PB2—PB2^xxxiii	3.615 (3)	O1—O1^liii	3.415 (12)
PB2—PB2^xxxiv	3.415 (7)	O1—O1^liv	3.392 (10)
PB2—PB2^xxxv	3.805 (7)	O1—O1^lv	3.054 (4)
PB2—PB2^xxxvi	3.805 (7)	O1—O1^lvi	3.054 (4)
PB2—PB2^xxxvii	3.615 (3)	O1—O1^lvii	3.054 (4)
PB2—PB2^xxxviii	3.415 (7)	O1—O1^lviii	3.054 (4)
PB2—PB2^xxxix	4.002 (14)	O1—O1^lix	3.392 (10)
PB2—PB2^xl	3.434 (6)	O1—O2	2.634 (7)
PB2—PB2^xli	3.434 (6)	O1—O2^i	2.449 (4)
PB2—PB2^xlii	3.822 (8)	O1—O2^ii	2.427 (5)
PB2—PB2^xliii	3.223 (13)	O1—O2^iii	2.449 (4)
PB2—PB2^xliv	3.822 (8)	O1—O2^iv	2.634 (7)
PB2—PB2^xlv	3.606 (3)	O1—O2^v	2.427 (5)
PB2—PB2^xlvi	3.606 (3)	O1—O2^li	3.397 (6)
PB2—PB2^xlvii	3.606 (3)	O1—O2^liii	3.182 (6)
PB2—P	3.860 (6)	O1—O2^liv	3.327 (8)
PB2—P^xii	4.250 (4)	O1—O2^lv	3.210 (8)
PB2—P^xiv	4.081 (7)	O1—O2^lviii	2.998 (9)
PB2—P^li	3.3458 (17)	O1—O2^lix	3.548 (10)
PB2—P^lii	3.550 (7)	O1—O2^lx	3.210 (8)
PB2—P^liii	3.128 (7)	O1—O2^lxi	3.327 (8)
PB2—O1	2.399 (6)	O1—O2^lxii	3.182 (6)
PB2—O1^i	2.355 (5)	O1—O2^lxiii	3.397 (6)
PB2—O1^ii	2.377 (5)	O1—O2^lxiv	3.548 (10)
PB2—O1^li	4.170 (5)	O1—O2^lxv	2.998 (9)
PB2—O1^lii	4.076 (9)	O2—PB1^xlix	2.572 (3)
PB2—O1^liii	3.997 (7)	O2—PB2^li	3.042 (8)
PB2—O1^liv	4.195 (6)	O2—PB2^liii	2.535 (7)
PB2—O1^lv	4.359 (9)	O2—PB2^liv	2.665 (10)
PB2—O1^lvi	3.742 (9)	O2—PB2^lvi	2.916 (10)
PB2—O1^lvii	3.913 (8)	O2—PB2^lvii	3.062 (8)
PB2—O1^lviii	4.347 (8)	O2—PB2^lix	2.559 (7)
PB2—O1^lix	4.010 (7)	O2—PB2^lxvi	3.170 (11)
PB2—O2^xiii	3.011 (5)	O2—PB2^lxi	2.412 (11)
PB2—O2^xvii	2.745 (6)	O2—PB2^lxii	2.789 (7)
PB2—O2^xviii	2.899 (3)	O2—PB2^lxiii	2.787 (7)
PB2—O2^xxi	2.875 (3)	O2—PB2^lxiv	2.811 (7)
PB2—O2^xxv	3.022 (5)	O2—PB2^lxviii	2.809 (7)
PB2—O2^xxvi	4.385 (8)	O2—PB2^xlix	3.011 (5)
PB2—O2^xxix	2.757 (6)	O2—PB2^lxix	2.899 (3)
PB2—O2^li	3.042 (8)	O2—PB2^lxxii	2.745 (6)
PB2—O2^liii	2.535 (7)	O2—PB2^lxxiv	2.875 (3)
PB2—O2^liv	2.559 (7)	O2—PB2^xcvii	3.022 (5)
PB2—O2^lv	3.062 (8)	O2—PB2^lxxvi	4.385 (8)
PB2—O2^lviii	2.916 (10)	O2—PB2^lxxvii	2.757 (6)
PB2—O2^lix	2.665 (10)	O2—P^xcviii	4.392 (5)
PB2—O2^lx	3.170 (11)	O2—P	1.541 (3)
PB2—O2^lxi	2.412 (11)	O2—P^xcix	4.227 (4)
PB2—O2^lxii	2.787 (7)	O2—P^lxxix	3.690 (5)
PB2—O2^lxiii	2.789 (7)	O2—P^li	4.366 (6)
PB2—O2^lxiv	2.811 (7)	O2—P^liii	4.201 (6)
PB2—O2^lxv	2.809 (7)	O2—O1	2.634 (7)
P—PB1^xlviii	3.4424 (19)	O2—O1^i	2.427 (5)
P—PB1^xlix	3.4424 (19)	O2—O1^ii	2.449 (4)
P—PB1^l	3.4424 (19)	O2—O1^li	3.397 (6)
P—PB2	3.860 (6)	O2—O1^liii	3.182 (6)
P—PB2^i	3.860 (6)	O2—O1^liv	3.548 (10)
P—PB2^ii	3.860 (6)	O2—O1^lvi	2.998 (9)
P—PB2^iii	3.860 (6)	O2—O1^lvii	3.210 (8)
P—PB2^iv	3.860 (6)	O2—O1^lix	3.327 (8)
P—PB2^v	3.860 (6)	O2—O2^i	2.504 (5)
P—PB2^li	3.3458 (17)	O2—O2^lxxxii	2.976 (5)
P—PB2^lii	3.550 (7)	O2—O2^lxxxv	2.976 (5)
P—PB2^liii	3.128 (7)	O2—O2^ii	2.504 (5)
P—PB2^liv	3.128 (7)	O2—O2^lxxxvii	3.097 (8)
P—PB2^lv	3.3458 (17)	O2—O2^iii	2.364 (8)
P—PB2^lvi	3.550 (7)	O2—O2^iv	0.259 (12)
P—PB2^lvii	3.550 (7)	O2—O2^v	2.624 (8)
P—PB2^lviii	3.128 (7)	O2—O2^xc	2.838 (8)
P—PB2^lix	3.3458 (17)	O2—O2^lxxix	4.068 (5)
P—PB2^lxvi	3.550 (7)	O2—O2^100	4.209 (8)
P—PB2^lx	3.3458 (17)	O2—O2^xcii	3.206 (5)
P—PB2^lxi	3.128 (7)	O2—O2^xciii	3.206 (5)
P—PB2^lxii	3.128 (7)	O2—O2^xciv	3.311 (7)
P—PB2^lxvii	3.550 (7)	O2—O2^101	4.367 (4)
P—PB2^lxiii	3.3458 (17)	O2—O2^xcv	4.060 (5)
P—PB2^lxiv	3.3458 (17)	O2—O2^102	4.367 (4)
P—PB2^lxv	3.128 (7)	O2—O2^xcvi	3.109 (6)
P—PB2^lxviii	3.550 (7)	O2—O2^liv	4.196 (5)
P—PB2^xlviii	4.081 (7)	O2—O2^lix	4.196 (5)
P—PB2^l	4.250 (4)	O2—O2^lxi	4.108 (6)
P—PB2^lxix	4.250 (4)	O2—O2^lxiv	4.291 (7)
PB2^i—PB2—PB2^ii	60.0000 (1)	O1^ii—P—O2	106.4 (2)
PB2^i—PB2—PB2^iii	90.0	O1^ii—P—O2^i	105.1 (3)
PB2^i—PB2—PB2^iv	30.0	O1^ii—P—O2^ii	118.9 (4)
PB2^i—PB2—PB2^v	30.0000 (1)	O1^ii—P—O2^iii	118.9 (4)
PB2^ii—PB2—PB2^iii	30.0	O1^ii—P—O2^iv	105.1 (3)
PB2^ii—PB2—PB2^iv	90.0	O1^ii—P—O2^v	106.4 (2)
PB2^ii—PB2—PB2^v	30.0000 (1)	O2—P—O2^i	108.70 (19)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	108.70 (19)
PB2^iii—PB2—PB2^v	60.0	O2—P—O2^iii	100.2 (4)
PB2^iv—PB2—PB2^v	60.0	O2—P—O2^iv	9.7 (5)
O1—P—O1^i	15.1 (6)	O2—P—O2^v	116.7 (5)
O1—P—O1^ii	15.1 (6)	O2^i—P—O2^ii	108.70 (19)
O1—P—O2	118.9 (4)	O2^i—P—O2^iii	116.7 (5)
O1—P—O2^i	106.4 (2)	O2^i—P—O2^iv	100.2 (4)
O1—P—O2^ii	105.1 (3)	O2^i—P—O2^v	9.7 (5)
O1—P—O2^iii	106.4 (2)	O2^ii—P—O2^iii	9.7 (5)
O1—P—O2^iv	118.9 (4)	O2^ii—P—O2^iv	116.7 (5)
O1—P—O2^v	105.1 (3)	O2^ii—P—O2^v	100.2 (4)
O1^i—P—O1^ii	15.1 (6)	O2^iii—P—O2^iv	108.70 (19)
O1^i—P—O2	105.1 (3)	O2^iii—P—O2^v	108.70 (19)
O1^i—P—O2^i	118.9 (4)	O2^iv—P—O2^v	108.70 (19)
O1^i—P—O2^ii	106.4 (2)	P—O1—O1^i	82.4 (3)
O1^i—P—O2^iii	105.1 (3)	P—O1—O1^ii	82.4 (3)
O1^i—P—O2^iv	106.4 (2)	O1^i—O1—O1^ii	60.0000 (2)
O1^i—P—O2^v	118.9 (4)	P—O2—O2^iv	85.2 (2)

Symmetry codes: (i) −y, x−y, z; (ii) y−x, −x, z; (iii) y−x, y, z; (iv) −y, −x, z; (v) x, x−y, z; (vi) −x, −y, −z; (vii) y, y−x, −z; (viii) x−y, x, −z; (ix) x−y, −y, −z; (x) y, x, −z; (xi) −x, y−x, −z; (xii) x−2/3, y−1/3, z−1/3; (xiii) x+1/3, y−1/3, z−1/3; (xiv) x+1/3, y+2/3, z−1/3; (xv) −y−2/3, x−y−1/3, z−1/3; (xvi) −y+1/3, x−y−1/3, z−1/3; (xvii) −y+1/3, x−y+2/3, z−1/3; (xviii) y−x−2/3, −x−1/3, z−1/3; (xix) y−x+1/3, −x−1/3, z−1/3; (xx) y−x+1/3, −x+2/3, z−1/3; (xxi) y−x−2/3, y−1/3, z−1/3; (xxii) y−x+1/3, y−1/3, z−1/3; (xxiii) y−x+1/3, y+2/3, z−1/3; (xxiv) −y−2/3, −x−1/3, z−1/3; (xxv) −y+1/3, −x−1/3, z−1/3; (xxvi) −y+1/3, −x+2/3, z−1/3; (xxvii) x−2/3, x−y−1/3, z−1/3; (xxviii) x+1/3, x−y−1/3, z−1/3; (xxix) x+1/3, x−y+2/3, z−1/3; (xxx) −x−2/3, −y−1/3, −z+2/3; (xxxi) −x−2/3, −y+2/3, −z+2/3; (xxxii) −x+1/3, −y+2/3, −z+2/3; (xxxiii) y−2/3, y−x−1/3, −z+2/3; (xxxiv) y−2/3, y−x+2/3, −z+2/3; (xxxv) y+1/3, y−x+2/3, −z+2/3; (xxxvi) x−y−2/3, x−1/3, −z+2/3; (xxxvii) x−y−2/3, x+2/3, −z+2/3; (xxxviii) x−y+1/3, x+2/3, −z+2/3; (xxxix) x−y−2/3, −y−1/3, −z+2/3; (xl) x−y−2/3, −y+2/3, −z+2/3; (xli) x−y+1/3, −y+2/3, −z+2/3; (xlii) y−2/3, x−1/3, −z+2/3; (xliii) y−2/3, x+2/3, −z+2/3; (xliv) y+1/3, x+2/3, −z+2/3; (xlv) −x−2/3, y−x−1/3, −z+2/3; (xlvi) −x−2/3, y−x+2/3, −z+2/3; (xlvii) −x+1/3, y−x+2/3, −z+2/3; (xlviii) x−1/3, y−2/3, z+1/3; (xlix) x−1/3, y+1/3, z+1/3; (l) x+2/3, y+1/3, z+1/3; (li) −x−1/3, −y−2/3, −z+1/3; (lii) −x+2/3, −y−2/3, −z+1/3; (liii) −x+2/3, −y+1/3, −z+1/3; (liv) y−1/3, y−x−2/3, −z+1/3; (lv) y+2/3, y−x−2/3, −z+1/3; (lvi) y+2/3, y−x+1/3, −z+1/3; (lvii) x−y−1/3, x−2/3, −z+1/3; (lviii) x−y+2/3, x−2/3, −z+1/3; (lix) x−y+2/3, x+1/3, −z+1/3; (lx) x−y+2/3, −y−2/3, −z+1/3; (lxi) x−y+2/3, −y+1/3, −z+1/3; (lxii) y−1/3, x−2/3, −z+1/3; (lxiii) y+2/3, x+1/3, −z+1/3; (lxiv) −x−1/3, y−x−2/3, −z+1/3; (lxv) −x+2/3, y−x−2/3, −z+1/3; (lxvi) x−y−1/3, −y−2/3, −z+1/3; (lxvii) y+2/3, x−2/3, −z+1/3; (lxviii) −x+2/3, y−x+1/3, −z+1/3; (lxix) −y−1/3, x−y+1/3, z+1/3; (lxx) −y+2/3, x−y+1/3, z+1/3; (lxxi) y−x−1/3, −x−2/3, z+1/3; (lxxii) y−x−1/3, −x+1/3, z+1/3; (lxxiii) y−x−1/3, y−2/3, z+1/3; (lxxiv) y−x−1/3, y+1/3, z+1/3; (lxxv) −y−1/3, −x−2/3, z+1/3; (lxxvi) −y+2/3, −x+1/3, z+1/3; (lxxvii) x−1/3, x−y+1/3, z+1/3; (lxxviii) x+2/3, x−y+1/3, z+1/3; (lxxix) −x, −y, −z+1; (lxxx) x, y−1, z; (lxxxi) x+1, y, z; (lxxxii) −y, x−y+1, z; (lxxxiii) −y+1, x−y+1, z; (lxxxiv) y−x−1, −x−1, z; (lxxxv) y−x−1, −x, z; (lxxxvi) y−x−1, y−1, z; (lxxxvii) y−x−1, y, z; (lxxxviii) −y, −x−1, z; (lxxxix) −y+1, −x, z; (xc) x, x−y+1, z; (xci) x+1, x−y+1, z; (xcii) y, y−x, −z+1; (xciii) x−y, x, −z+1; (xciv) x−y, −y, −z+1; (xcv) y, x, −z+1; (xcvi) −x, y−x, −z+1; (xcvii) −y−1/3, −x+1/3, z+1/3; (xcviii) x−1, y, z; (xcix) x, y+1, z; (100) −x, −y+1, −z+1; (101) y−1, x, −z+1; (102) y, x+1, −z+1.

(S2P19D_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8974 (6) Å	T = 298 K
c = 2.8295 (10) Å	Particle morphology: Pressure cell anvil material
V = 20.57 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.883 < d <3.007 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 90.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 9.23 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 128.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 241.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.044	36 parameters
Rexp = 0.039	9 restraints
R(F^2) = 0.18408	(Δ/σ)max = 0.01
χ^2 = 1.277	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.505026 2: -3.751250E-03 3: 0.259623 4: -2.540250E-02 5: 7.578030E-02 6: -4.593390E-02 7: 4.408820E-02 8: -2.570450E-02 9: 4.284580E-0210: -1.657270E-0211: 1.488630E-0212: -5.843410E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89345 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.228 (3)	P—PB2	4.081 (7)
PB1—PB2^i	4.228 (3)	P—PB2	4.250 (4)
PB1—PB2^ii	4.228 (3)	P—PB2	4.081 (7)
PB1—PB2^iii	4.228 (3)	P—PB2	4.081 (7)
PB1—PB2^iv	4.228 (3)	P—PB2	4.250 (4)
PB1—PB2^v	4.228 (3)	P—PB2	4.250 (4)
PB1—PB2	4.228 (3)	P—PB2	4.081 (7)
PB1—PB2	4.228 (3)	P—PB2	4.081 (7)
PB1—PB2	4.228 (3)	P—PB2	4.250 (4)
PB1—PB2	4.228 (3)	P—P	3.928 (9)
PB1—PB2	4.228 (3)	P—P	4.192 (6)
PB1—PB2	4.228 (3)	P—P	4.192 (6)
PB1—PB2	4.014 (2)	P—P	4.192 (6)
PB1—PB2	3.834 (6)	P—O1	1.518 (5)
PB1—PB2	4.186 (6)	P—O1^i	1.518 (5)
PB1—PB2	4.186 (6)	P—O1^ii	1.518 (5)
PB1—PB2	4.014 (2)	P—O1	3.510 (6)
PB1—PB2	3.834 (6)	P—O1	3.184 (9)
PB1—PB2	3.834 (6)	P—O1	3.510 (6)
PB1—PB2	4.186 (6)	P—O1	3.510 (6)
PB1—PB2	4.014 (2)	P—O1	3.510 (6)
PB1—PB2	3.834 (6)	P—O1	3.184 (9)
PB1—PB2	4.014 (2)	P—O1	3.184 (9)
PB1—PB2	4.186 (6)	P—O1	3.510 (6)
PB1—PB2	4.186 (6)	P—O1	3.510 (6)
PB1—PB2	3.834 (6)	P—O2^vi	4.227 (4)
PB1—PB2	4.014 (2)	P—O2	1.541 (3)
PB1—PB2	4.014 (2)	P—O2^vii	4.392 (5)
PB1—PB2	4.186 (6)	P—O2^i	1.541 (3)
PB1—PB2	3.834 (6)	P—O2^viii	4.392 (5)
PB1—PB2	4.186 (6)	P—O2^ix	4.227 (4)
PB1—PB2	3.834 (6)	P—O2^x	4.392 (5)
PB1—PB2	4.014 (2)	P—O2^xi	4.227 (4)
PB1—PB2	3.834 (6)	P—O2^ii	1.541 (3)
PB1—PB2	4.014 (2)	P—O2^xii	4.227 (4)
PB1—PB2	4.186 (6)	P—O2^xiii	4.392 (5)
PB1—PB2	4.014 (2)	P—O2^iii	1.541 (3)
PB1—PB2	4.186 (6)	P—O2^xiv	4.392 (5)
PB1—PB2	3.834 (6)	P—O2^iv	1.541 (3)
PB1—PB2	4.186 (6)	P—O2^xv	4.227 (4)
PB1—PB2	4.014 (2)	P—O2^v	1.541 (3)
PB1—PB2	3.834 (6)	P—O2^xvi	4.227 (4)
PB1—PB2	4.014 (2)	P—O2^xvii	4.392 (5)
PB1—PB2	3.834 (6)	P—O2	3.690 (5)
PB1—PB2	4.186 (6)	P—O2	3.690 (5)
PB1—PB2	3.834 (6)	P—O2	3.690 (5)
PB1—PB2	4.186 (6)	P—O2	3.690 (5)
PB1—PB2	4.014 (2)	P—O2	3.690 (5)
PB1—P	3.4424 (19)	P—O2	3.690 (5)
PB1—P	3.4424 (19)	P—O2	4.366 (6)
PB1—P	3.4424 (19)	P—O2	4.201 (6)
PB1—P	3.4424 (19)	P—O2	4.201 (6)
PB1—P	3.4424 (19)	P—O2	4.366 (6)
PB1—P	3.4424 (19)	P—O2	4.201 (6)
PB1—O1	3.047 (4)	P—O2	4.366 (6)
PB1—O1	3.386 (10)	P—O2	4.366 (6)
PB1—O1	3.047 (4)	P—O2	4.201 (6)
PB1—O1	3.047 (4)	P—O2	4.201 (6)
PB1—O1	3.047 (4)	P—O2	4.366 (6)
PB1—O1	3.386 (10)	P—O2	4.366 (6)
PB1—O1	3.386 (10)	P—O2	4.201 (6)
PB1—O1	3.047 (4)	O1—PB1	3.047 (4)
PB1—O1	3.047 (4)	O1—PB1	3.386 (10)
PB1—O1	3.047 (4)	O1—PB1	3.047 (4)
PB1—O1	3.386 (10)	O1—PB2	2.399 (6)
PB1—O1	3.047 (4)	O1—PB2^i	2.377 (5)
PB1—O1	3.386 (10)	O1—PB2^ii	2.355 (5)
PB1—O1	3.047 (4)	O1—PB2^iii	2.377 (5)
PB1—O1	3.047 (4)	O1—PB2^iv	2.399 (6)
PB1—O1	3.047 (4)	O1—PB2^v	2.355 (5)
PB1—O1	3.047 (4)	O1—PB2	4.170 (5)
PB1—O1	3.386 (10)	O1—PB2	4.076 (9)
PB1—O2	2.572 (3)	O1—PB2	3.997 (7)
PB1—O2	2.572 (3)	O1—PB2	4.010 (7)
PB1—O2	2.572 (3)	O1—PB2	3.913 (8)
PB1—O2	2.572 (3)	O1—PB2	4.347 (8)
PB1—O2	2.572 (3)	O1—PB2	4.359 (9)
PB1—O2	2.572 (3)	O1—PB2	3.742 (9)
PB1—O2	2.572 (3)	O1—PB2	4.195 (6)
PB1—O2	2.572 (3)	O1—PB2	4.347 (8)
PB1—O2	2.572 (3)	O1—PB2	3.913 (8)
PB1—O2	2.572 (3)	O1—PB2	4.010 (7)
PB1—O2	2.572 (3)	O1—PB2	3.997 (7)
PB1—O2	2.572 (3)	O1—PB2	4.076 (9)
PB2—PB1	4.228 (3)	O1—PB2	4.170 (5)
PB2—PB1	4.186 (6)	O1—PB2	4.195 (6)
PB2—PB1	3.834 (6)	O1—PB2	3.742 (9)
PB2—PB1	4.014 (2)	O1—PB2	4.359 (9)
PB2—PB2^i	0.447 (15)	O1—P	1.518 (5)
PB2—PB2^ii	0.447 (15)	O1—P	3.510 (6)
PB2—PB2^iii	0.258 (9)	O1—P	3.184 (9)
PB2—PB2^iv	0.258 (9)	O1—P	3.510 (6)
PB2—PB2^v	0.516 (17)	O1—O1^i	0.399 (17)
PB2—PB2	4.011 (14)	O1—O1^ii	0.399 (17)
PB2—PB2	3.233 (12)	O1—O1	3.415 (12)
PB2—PB2	3.643 (4)	O1—O1	2.702 (19)
PB2—PB2	3.615 (3)	O1—O1	3.415 (12)
PB2—PB2	3.415 (7)	O1—O1	3.392 (10)
PB2—PB2	3.805 (7)	O1—O1	3.054 (4)
PB2—PB2	3.805 (7)	O1—O1	3.054 (4)
PB2—PB2	3.615 (3)	O1—O1	3.054 (4)
PB2—PB2	3.415 (7)	O1—O1	3.054 (4)
PB2—PB2	4.002 (14)	O1—O1	3.392 (10)
PB2—PB2	3.434 (6)	O1—O2	2.634 (7)
PB2—PB2	3.434 (6)	O1—O2^i	2.449 (4)
PB2—PB2	3.822 (8)	O1—O2^ii	2.427 (5)
PB2—PB2	3.223 (13)	O1—O2^iii	2.449 (4)
PB2—PB2	3.822 (8)	O1—O2^iv	2.634 (7)
PB2—PB2	3.606 (3)	O1—O2^v	2.427 (5)
PB2—PB2	3.606 (3)	O1—O2	3.397 (6)
PB2—PB2	3.606 (3)	O1—O2	3.182 (6)
PB2—P	3.860 (6)	O1—O2	3.327 (8)
PB2—P	4.250 (4)	O1—O2	3.210 (8)
PB2—P	4.081 (7)	O1—O2	2.998 (9)
PB2—P	3.3458 (17)	O1—O2	3.548 (10)
PB2—P	3.550 (7)	O1—O2	3.210 (8)
PB2—P	3.128 (7)	O1—O2	3.327 (8)
PB2—O1	2.399 (6)	O1—O2	3.182 (6)
PB2—O1^i	2.355 (5)	O1—O2	3.397 (6)
PB2—O1^ii	2.377 (5)	O1—O2	3.548 (10)
PB2—O1	4.170 (5)	O1—O2	2.998 (9)
PB2—O1	4.076 (9)	O2—PB1	2.572 (3)
PB2—O1	3.997 (7)	O2—PB2	3.042 (8)
PB2—O1	4.195 (6)	O2—PB2	2.535 (7)
PB2—O1	4.359 (9)	O2—PB2	2.665 (10)
PB2—O1	3.742 (9)	O2—PB2	2.916 (10)
PB2—O1	3.913 (8)	O2—PB2	3.062 (8)
PB2—O1	4.347 (8)	O2—PB2	2.559 (7)
PB2—O1	4.010 (7)	O2—PB2	3.170 (11)
PB2—O2	3.011 (5)	O2—PB2	2.412 (11)
PB2—O2	2.745 (6)	O2—PB2	2.789 (7)
PB2—O2	2.899 (3)	O2—PB2	2.787 (7)
PB2—O2	2.875 (3)	O2—PB2	2.811 (7)
PB2—O2	3.022 (5)	O2—PB2	2.809 (7)
PB2—O2	4.385 (8)	O2—PB2	3.011 (5)
PB2—O2	2.757 (6)	O2—PB2	2.899 (3)
PB2—O2	3.042 (8)	O2—PB2	2.745 (6)
PB2—O2	2.535 (7)	O2—PB2	2.875 (3)
PB2—O2	2.559 (7)	O2—PB2	3.022 (5)
PB2—O2	3.062 (8)	O2—PB2	4.385 (8)
PB2—O2	2.916 (10)	O2—PB2	2.757 (6)
PB2—O2	2.665 (10)	O2—P^xviii	4.392 (5)
PB2—O2	3.170 (11)	O2—P	1.541 (3)
PB2—O2	2.412 (11)	O2—P^xix	4.227 (4)
PB2—O2	2.787 (7)	O2—P	3.690 (5)
PB2—O2	2.789 (7)	O2—P	4.366 (6)
PB2—O2	2.811 (7)	O2—P	4.201 (6)
PB2—O2	2.809 (7)	O2—O1	2.634 (7)
P—PB1	3.4424 (19)	O2—O1^i	2.427 (5)
P—PB1	3.4424 (19)	O2—O1^ii	2.449 (4)
P—PB1	3.4424 (19)	O2—O1	3.397 (6)
P—PB2	3.860 (6)	O2—O1	3.182 (6)
P—PB2^i	3.860 (6)	O2—O1	3.548 (10)
P—PB2^ii	3.860 (6)	O2—O1	2.998 (9)
P—PB2^iii	3.860 (6)	O2—O1	3.210 (8)
P—PB2^iv	3.860 (6)	O2—O1	3.327 (8)
P—PB2^v	3.860 (6)	O2—O2^i	2.504 (5)
P—PB2	3.3458 (17)	O2—O2^viii	2.976 (5)
P—PB2	3.550 (7)	O2—O2^xi	2.976 (5)
P—PB2	3.128 (7)	O2—O2^ii	2.504 (5)
P—PB2	3.128 (7)	O2—O2^xiii	3.097 (8)
P—PB2	3.3458 (17)	O2—O2^iii	2.364 (8)
P—PB2	3.550 (7)	O2—O2^iv	0.259 (12)
P—PB2	3.550 (7)	O2—O2^v	2.624 (8)
P—PB2	3.128 (7)	O2—O2^xvi	2.838 (8)
P—PB2	3.3458 (17)	O2—O2	4.068 (5)
P—PB2	3.550 (7)	O2—O2	4.209 (8)
P—PB2	3.3458 (17)	O2—O2	3.206 (5)
P—PB2	3.128 (7)	O2—O2	3.206 (5)
P—PB2	3.128 (7)	O2—O2	3.311 (7)
P—PB2	3.550 (7)	O2—O2	4.367 (4)
P—PB2	3.3458 (17)	O2—O2	4.060 (5)
P—PB2	3.3458 (17)	O2—O2	4.367 (4)
P—PB2	3.128 (7)	O2—O2	3.109 (6)
P—PB2	3.550 (7)	O2—O2	4.196 (5)
P—PB2	4.081 (7)	O2—O2	4.196 (5)
P—PB2	4.250 (4)	O2—O2	4.108 (6)
P—PB2	4.250 (4)	O2—O2	4.291 (7)
PB2^i—PB2—PB2^ii	60.0000 (1)	O1^ii—P—O2	106.4 (2)
PB2^i—PB2—PB2^iii	90.0	O1^ii—P—O2^i	105.1 (3)
PB2^i—PB2—PB2^iv	30.0	O1^ii—P—O2^ii	118.9 (4)
PB2^i—PB2—PB2^v	30.0000 (1)	O1^ii—P—O2^iii	118.9 (4)
PB2^ii—PB2—PB2^iii	30.0	O1^ii—P—O2^iv	105.1 (3)
PB2^ii—PB2—PB2^iv	90.0	O1^ii—P—O2^v	106.4 (2)
PB2^ii—PB2—PB2^v	30.0000 (1)	O2—P—O2^i	108.70 (19)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	108.70 (19)
PB2^iii—PB2—PB2^v	60.0	O2—P—O2^iii	100.2 (4)
PB2^iv—PB2—PB2^v	60.0	O2—P—O2^iv	9.7 (5)
O1—P—O1^i	15.1 (6)	O2—P—O2^v	116.7 (5)
O1—P—O1^ii	15.1 (6)	O2^i—P—O2^ii	108.70 (19)
O1—P—O2	118.9 (4)	O2^i—P—O2^iii	116.7 (5)
O1—P—O2^i	106.4 (2)	O2^i—P—O2^iv	100.2 (4)
O1—P—O2^ii	105.1 (3)	O2^i—P—O2^v	9.7 (5)
O1—P—O2^iii	106.4 (2)	O2^ii—P—O2^iii	9.7 (5)
O1—P—O2^iv	118.9 (4)	O2^ii—P—O2^iv	116.7 (5)
O1—P—O2^v	105.1 (3)	O2^ii—P—O2^v	100.2 (4)
O1^i—P—O1^ii	15.1 (6)	O2^iii—P—O2^iv	108.70 (19)
O1^i—P—O2	105.1 (3)	O2^iii—P—O2^v	108.70 (19)
O1^i—P—O2^i	118.9 (4)	O2^iv—P—O2^v	108.70 (19)
O1^i—P—O2^ii	106.4 (2)	P—O1—O1^i	82.4 (3)
O1^i—P—O2^iii	105.1 (3)	P—O1—O1^ii	82.4 (3)
O1^i—P—O2^iv	106.4 (2)	O1^i—O1—O1^ii	60.0000 (2)
O1^i—P—O2^v	118.9 (4)	P—O2—O2^iv	85.2 (2)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) x, y, −z; (iv) y−x, −x, z; (v) −y, x−y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) y−x, −x+1, −z; (ix) y−x+1, −x+1, −z; (x) −y−1, x−y−1, z; (xi) −y−1, x−y, z; (xii) x−1, y−1, −z; (xiii) x−1, y, −z; (xiv) y−x, −x−1, z; (xv) y−x+1, −x, z; (xvi) −y, x−y+1, −z; (xvii) −y+1, x−y+1, −z; (xviii) x−1, y, z; (xix) x, y+1, z.

(S2P19D_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5543 (6) Å	Particle morphology: Component of pressure cell, not sample
V = 44.90 (2) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.883 < d <3.007 Angstrom (contamination from unidentified phase), d > 3.625 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 90.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 9.23 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 128.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 241.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.044	36 parameters
Rexp = 0.039	9 restraints
R(F^2) = 0.18408	(Δ/σ)max = 0.01
χ^2 = 1.277	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 0.505026 2: -3.751250E-03 3: 0.259623 4: -2.540250E-02 5: 7.578030E-02 6: -4.593390E-02 7: 4.408820E-02 8: -2.570450E-02 9: 4.284580E-0210: -1.657270E-0211: 1.488630E-0212: -5.843410E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.89345 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.228 (3)	P—PB2^lxx	4.081 (7)
PB1—PB2^i	4.228 (3)	P—PB2^lxxi	4.250 (4)
PB1—PB2^ii	4.228 (3)	P—PB2^lxxii	4.081 (7)
PB1—PB2^iii	4.228 (3)	P—PB2^lxxiii	4.081 (7)
PB1—PB2^iv	4.228 (3)	P—PB2^lxxiv	4.250 (4)
PB1—PB2^v	4.228 (3)	P—PB2^lxxv	4.250 (4)
PB1—PB2^vi	4.228 (3)	P—PB2^lxxvi	4.081 (7)
PB1—PB2^vii	4.228 (3)	P—PB2^lxxvii	4.081 (7)
PB1—PB2^viii	4.228 (3)	P—PB2^lxxviii	4.250 (4)
PB1—PB2^ix	4.228 (3)	P—P^lxxix	3.928 (9)
PB1—PB2^x	4.228 (3)	P—P^li	4.192 (6)
PB1—PB2^xi	4.228 (3)	P—P^lii	4.192 (6)
PB1—PB2^xii	4.014 (2)	P—P^liii	4.192 (6)
PB1—PB2^xiii	3.834 (6)	P—O1	1.518 (5)
PB1—PB2^xiv	4.186 (6)	P—O1^i	1.518 (5)
PB1—PB2^xv	4.186 (6)	P—O1^ii	1.518 (5)
PB1—PB2^xvi	4.014 (2)	P—O1^li	3.510 (6)
PB1—PB2^xvii	3.834 (6)	P—O1^lii	3.184 (9)
PB1—PB2^xviii	3.834 (6)	P—O1^liii	3.510 (6)
PB1—PB2^xix	4.186 (6)	P—O1^liv	3.510 (6)
PB1—PB2^xx	4.014 (2)	P—O1^lv	3.510 (6)
PB1—PB2^xxi	3.834 (6)	P—O1^lvi	3.184 (9)
PB1—PB2^xxii	4.014 (2)	P—O1^lvii	3.184 (9)
PB1—PB2^xxiii	4.186 (6)	P—O1^lviii	3.510 (6)
PB1—PB2^xxiv	4.186 (6)	P—O1^lix	3.510 (6)
PB1—PB2^xxv	3.834 (6)	P—O2^lxxx	4.227 (4)
PB1—PB2^xxvi	4.014 (2)	P—O2	1.541 (3)
PB1—PB2^xxvii	4.014 (2)	P—O2^lxxxi	4.392 (5)
PB1—PB2^xxviii	4.186 (6)	P—O2^i	1.541 (3)
PB1—PB2^xxix	3.834 (6)	P—O2^lxxxii	4.392 (5)
PB1—PB2^xxx	4.186 (6)	P—O2^lxxxiii	4.227 (4)
PB1—PB2^xxxi	3.834 (6)	P—O2^lxxxiv	4.392 (5)
PB1—PB2^xxxii	4.014 (2)	P—O2^lxxxv	4.227 (4)
PB1—PB2^xxxiii	3.834 (6)	P—O2^ii	1.541 (3)
PB1—PB2^xxxiv	4.014 (2)	P—O2^lxxxvi	4.227 (4)
PB1—PB2^xxxv	4.186 (6)	P—O2^lxxxvii	4.392 (5)
PB1—PB2^xxxvi	4.014 (2)	P—O2^iii	1.541 (3)
PB1—PB2^xxxvii	4.186 (6)	P—O2^lxxxviii	4.392 (5)
PB1—PB2^xxxviii	3.834 (6)	P—O2^iv	1.541 (3)
PB1—PB2^xxxix	4.186 (6)	P—O2^lxxxix	4.227 (4)
PB1—PB2^xl	4.014 (2)	P—O2^v	1.541 (3)
PB1—PB2^xli	3.834 (6)	P—O2^xc	4.227 (4)
PB1—PB2^xlii	4.014 (2)	P—O2^xci	4.392 (5)
PB1—PB2^xliii	3.834 (6)	P—O2^lxxix	3.690 (5)
PB1—PB2^xliv	4.186 (6)	P—O2^xcii	3.690 (5)
PB1—PB2^xlv	3.834 (6)	P—O2^xciii	3.690 (5)
PB1—PB2^xlvi	4.186 (6)	P—O2^xciv	3.690 (5)
PB1—PB2^xlvii	4.014 (2)	P—O2^xcv	3.690 (5)
PB1—P^xii	3.4424 (19)	P—O2^xcvi	3.690 (5)
PB1—P^xiii	3.4424 (19)	P—O2^li	4.366 (6)
PB1—P^xiv	3.4424 (19)	P—O2^liii	4.201 (6)
PB1—P^xxx	3.4424 (19)	P—O2^liv	4.201 (6)
PB1—P^xxxi	3.4424 (19)	P—O2^lv	4.366 (6)
PB1—P^xxxii	3.4424 (19)	P—O2^lviii	4.201 (6)
PB1—O1^xii	3.047 (4)	P—O2^lix	4.366 (6)
PB1—O1^xiii	3.386 (10)	P—O2^lx	4.366 (6)
PB1—O1^xiv	3.047 (4)	P—O2^lxi	4.201 (6)
PB1—O1^xv	3.047 (4)	P—O2^lxii	4.201 (6)
PB1—O1^xvi	3.047 (4)	P—O2^lxiii	4.366 (6)
PB1—O1^xvii	3.386 (10)	P—O2^lxiv	4.366 (6)
PB1—O1^xviii	3.386 (10)	P—O2^lxv	4.201 (6)
PB1—O1^xix	3.047 (4)	O1—PB1^xlviii	3.047 (4)
PB1—O1^xx	3.047 (4)	O1—PB1^xlix	3.386 (10)
PB1—O1^xxx	3.047 (4)	O1—PB1^l	3.047 (4)
PB1—O1^xxxi	3.386 (10)	O1—PB2	2.399 (6)
PB1—O1^xxxii	3.047 (4)	O1—PB2^i	2.377 (5)
PB1—O1^xxxiii	3.386 (10)	O1—PB2^ii	2.355 (5)
PB1—O1^xxxiv	3.047 (4)	O1—PB2^iii	2.377 (5)
PB1—O1^xxxv	3.047 (4)	O1—PB2^iv	2.399 (6)
PB1—O1^xxxvi	3.047 (4)	O1—PB2^v	2.355 (5)
PB1—O1^xxxvii	3.047 (4)	O1—PB2^li	4.170 (5)
PB1—O1^xxxviii	3.386 (10)	O1—PB2^lii	4.076 (9)
PB1—O2^xiii	2.572 (3)	O1—PB2^liii	3.997 (7)
PB1—O2^xvii	2.572 (3)	O1—PB2^liv	4.010 (7)
PB1—O2^xviii	2.572 (3)	O1—PB2^lv	3.913 (8)
PB1—O2^xxi	2.572 (3)	O1—PB2^lvi	4.347 (8)
PB1—O2^xxv	2.572 (3)	O1—PB2^lvii	4.359 (9)
PB1—O2^xxix	2.572 (3)	O1—PB2^lviii	3.742 (9)
PB1—O2^xxxi	2.572 (3)	O1—PB2^lix	4.195 (6)
PB1—O2^xxxiii	2.572 (3)	O1—PB2^lxvi	4.347 (8)
PB1—O2^xxxviii	2.572 (3)	O1—PB2^lx	3.913 (8)
PB1—O2^xli	2.572 (3)	O1—PB2^lxi	4.010 (7)
PB1—O2^xliii	2.572 (3)	O1—PB2^lxii	3.997 (7)
PB1—O2^xlv	2.572 (3)	O1—PB2^lxvii	4.076 (9)
PB2—PB1	4.228 (3)	O1—PB2^lxiii	4.170 (5)
PB2—PB1^xlviii	4.186 (6)	O1—PB2^lxiv	4.195 (6)
PB2—PB1^xlix	3.834 (6)	O1—PB2^lxv	3.742 (9)
PB2—PB1^l	4.014 (2)	O1—PB2^lxviii	4.359 (9)
PB2—PB2^i	0.447 (15)	O1—P	1.518 (5)
PB2—PB2^ii	0.447 (15)	O1—P^li	3.510 (6)
PB2—PB2^iii	0.258 (9)	O1—P^lii	3.184 (9)
PB2—PB2^iv	0.258 (9)	O1—P^liii	3.510 (6)
PB2—PB2^v	0.516 (17)	O1—O1^i	0.399 (17)
PB2—PB2^xxx	4.011 (14)	O1—O1^ii	0.399 (17)
PB2—PB2^xxxi	3.233 (12)	O1—O1^li	3.415 (12)
PB2—PB2^xxxii	3.643 (4)	O1—O1^lii	2.702 (19)
PB2—PB2^xxxiii	3.615 (3)	O1—O1^liii	3.415 (12)
PB2—PB2^xxxiv	3.415 (7)	O1—O1^liv	3.392 (10)
PB2—PB2^xxxv	3.805 (7)	O1—O1^lv	3.054 (4)
PB2—PB2^xxxvi	3.805 (7)	O1—O1^lvi	3.054 (4)
PB2—PB2^xxxvii	3.615 (3)	O1—O1^lvii	3.054 (4)
PB2—PB2^xxxviii	3.415 (7)	O1—O1^lviii	3.054 (4)
PB2—PB2^xxxix	4.002 (14)	O1—O1^lix	3.392 (10)
PB2—PB2^xl	3.434 (6)	O1—O2	2.634 (7)
PB2—PB2^xli	3.434 (6)	O1—O2^i	2.449 (4)
PB2—PB2^xlii	3.822 (8)	O1—O2^ii	2.427 (5)
PB2—PB2^xliii	3.223 (13)	O1—O2^iii	2.449 (4)
PB2—PB2^xliv	3.822 (8)	O1—O2^iv	2.634 (7)
PB2—PB2^xlv	3.606 (3)	O1—O2^v	2.427 (5)
PB2—PB2^xlvi	3.606 (3)	O1—O2^li	3.397 (6)
PB2—PB2^xlvii	3.606 (3)	O1—O2^liii	3.182 (6)
PB2—P	3.860 (6)	O1—O2^liv	3.327 (8)
PB2—P^xii	4.250 (4)	O1—O2^lv	3.210 (8)
PB2—P^xiv	4.081 (7)	O1—O2^lviii	2.998 (9)
PB2—P^li	3.3458 (17)	O1—O2^lix	3.548 (10)
PB2—P^lii	3.550 (7)	O1—O2^lx	3.210 (8)
PB2—P^liii	3.128 (7)	O1—O2^lxi	3.327 (8)
PB2—O1	2.399 (6)	O1—O2^lxii	3.182 (6)
PB2—O1^i	2.355 (5)	O1—O2^lxiii	3.397 (6)
PB2—O1^ii	2.377 (5)	O1—O2^lxiv	3.548 (10)
PB2—O1^li	4.170 (5)	O1—O2^lxv	2.998 (9)
PB2—O1^lii	4.076 (9)	O2—PB1^xlix	2.572 (3)
PB2—O1^liii	3.997 (7)	O2—PB2^li	3.042 (8)
PB2—O1^liv	4.195 (6)	O2—PB2^liii	2.535 (7)
PB2—O1^lv	4.359 (9)	O2—PB2^liv	2.665 (10)
PB2—O1^lvi	3.742 (9)	O2—PB2^lvi	2.916 (10)
PB2—O1^lvii	3.913 (8)	O2—PB2^lvii	3.062 (8)
PB2—O1^lviii	4.347 (8)	O2—PB2^lix	2.559 (7)
PB2—O1^lix	4.010 (7)	O2—PB2^lxvi	3.170 (11)
PB2—O2^xiii	3.011 (5)	O2—PB2^lxi	2.412 (11)
PB2—O2^xvii	2.745 (6)	O2—PB2^lxii	2.789 (7)
PB2—O2^xviii	2.899 (3)	O2—PB2^lxiii	2.787 (7)
PB2—O2^xxi	2.875 (3)	O2—PB2^lxiv	2.811 (7)
PB2—O2^xxv	3.022 (5)	O2—PB2^lxviii	2.809 (7)
PB2—O2^xxvi	4.385 (8)	O2—PB2^xlix	3.011 (5)
PB2—O2^xxix	2.757 (6)	O2—PB2^lxix	2.899 (3)
PB2—O2^li	3.042 (8)	O2—PB2^lxxii	2.745 (6)
PB2—O2^liii	2.535 (7)	O2—PB2^lxxiv	2.875 (3)
PB2—O2^liv	2.559 (7)	O2—PB2^xcvii	3.022 (5)
PB2—O2^lv	3.062 (8)	O2—PB2^lxxvi	4.385 (8)
PB2—O2^lviii	2.916 (10)	O2—PB2^lxxvii	2.757 (6)
PB2—O2^lix	2.665 (10)	O2—P^xcviii	4.392 (5)
PB2—O2^lx	3.170 (11)	O2—P	1.541 (3)
PB2—O2^lxi	2.412 (11)	O2—P^xcix	4.227 (4)
PB2—O2^lxii	2.787 (7)	O2—P^lxxix	3.690 (5)
PB2—O2^lxiii	2.789 (7)	O2—P^li	4.366 (6)
PB2—O2^lxiv	2.811 (7)	O2—P^liii	4.201 (6)
PB2—O2^lxv	2.809 (7)	O2—O1	2.634 (7)
P—PB1^xlviii	3.4424 (19)	O2—O1^i	2.427 (5)
P—PB1^xlix	3.4424 (19)	O2—O1^ii	2.449 (4)
P—PB1^l	3.4424 (19)	O2—O1^li	3.397 (6)
P—PB2	3.860 (6)	O2—O1^liii	3.182 (6)
P—PB2^i	3.860 (6)	O2—O1^liv	3.548 (10)
P—PB2^ii	3.860 (6)	O2—O1^lvi	2.998 (9)
P—PB2^iii	3.860 (6)	O2—O1^lvii	3.210 (8)
P—PB2^iv	3.860 (6)	O2—O1^lix	3.327 (8)
P—PB2^v	3.860 (6)	O2—O2^i	2.504 (5)
P—PB2^li	3.3458 (17)	O2—O2^lxxxii	2.976 (5)
P—PB2^lii	3.550 (7)	O2—O2^lxxxv	2.976 (5)
P—PB2^liii	3.128 (7)	O2—O2^ii	2.504 (5)
P—PB2^liv	3.128 (7)	O2—O2^lxxxvii	3.097 (8)
P—PB2^lv	3.3458 (17)	O2—O2^iii	2.364 (8)
P—PB2^lvi	3.550 (7)	O2—O2^iv	0.259 (12)
P—PB2^lvii	3.550 (7)	O2—O2^v	2.624 (8)
P—PB2^lviii	3.128 (7)	O2—O2^xc	2.838 (8)
P—PB2^lix	3.3458 (17)	O2—O2^lxxix	4.068 (5)
P—PB2^lxvi	3.550 (7)	O2—O2^100	4.209 (8)
P—PB2^lx	3.3458 (17)	O2—O2^xcii	3.206 (5)
P—PB2^lxi	3.128 (7)	O2—O2^xciii	3.206 (5)
P—PB2^lxii	3.128 (7)	O2—O2^xciv	3.311 (7)
P—PB2^lxvii	3.550 (7)	O2—O2^101	4.367 (4)
P—PB2^lxiii	3.3458 (17)	O2—O2^xcv	4.060 (5)
P—PB2^lxiv	3.3458 (17)	O2—O2^102	4.367 (4)
P—PB2^lxv	3.128 (7)	O2—O2^xcvi	3.109 (6)
P—PB2^lxviii	3.550 (7)	O2—O2^liv	4.196 (5)
P—PB2^xlviii	4.081 (7)	O2—O2^lix	4.196 (5)
P—PB2^l	4.250 (4)	O2—O2^lxi	4.108 (6)
P—PB2^lxix	4.250 (4)	O2—O2^lxiv	4.291 (7)
PB2^i—PB2—PB2^ii	60.0000 (1)	O1^ii—P—O2	106.4 (2)
PB2^i—PB2—PB2^iii	90.0	O1^ii—P—O2^i	105.1 (3)
PB2^i—PB2—PB2^iv	30.0	O1^ii—P—O2^ii	118.9 (4)
PB2^i—PB2—PB2^v	30.0000 (1)	O1^ii—P—O2^iii	118.9 (4)
PB2^ii—PB2—PB2^iii	30.0	O1^ii—P—O2^iv	105.1 (3)
PB2^ii—PB2—PB2^iv	90.0	O1^ii—P—O2^v	106.4 (2)
PB2^ii—PB2—PB2^v	30.0000 (1)	O2—P—O2^i	108.70 (19)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	108.70 (19)
PB2^iii—PB2—PB2^v	60.0	O2—P—O2^iii	100.2 (4)
PB2^iv—PB2—PB2^v	60.0	O2—P—O2^iv	9.7 (5)
O1—P—O1^i	15.1 (6)	O2—P—O2^v	116.7 (5)
O1—P—O1^ii	15.1 (6)	O2^i—P—O2^ii	108.70 (19)
O1—P—O2	118.9 (4)	O2^i—P—O2^iii	116.7 (5)
O1—P—O2^i	106.4 (2)	O2^i—P—O2^iv	100.2 (4)
O1—P—O2^ii	105.1 (3)	O2^i—P—O2^v	9.7 (5)
O1—P—O2^iii	106.4 (2)	O2^ii—P—O2^iii	9.7 (5)
O1—P—O2^iv	118.9 (4)	O2^ii—P—O2^iv	116.7 (5)
O1—P—O2^v	105.1 (3)	O2^ii—P—O2^v	100.2 (4)
O1^i—P—O1^ii	15.1 (6)	O2^iii—P—O2^iv	108.70 (19)
O1^i—P—O2	105.1 (3)	O2^iii—P—O2^v	108.70 (19)
O1^i—P—O2^i	118.9 (4)	O2^iv—P—O2^v	108.70 (19)
O1^i—P—O2^ii	106.4 (2)	P—O1—O1^i	82.4 (3)
O1^i—P—O2^iii	105.1 (3)	P—O1—O1^ii	82.4 (3)
O1^i—P—O2^iv	106.4 (2)	O1^i—O1—O1^ii	60.0000 (2)
O1^i—P—O2^v	118.9 (4)	P—O2—O2^iv	85.2 (2)

Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) x, y, −z; (iv) −z, x, y; (v) y, −z, x; (vi) −x, −y, −z; (vii) −z, −x, −y; (viii) −y, −z, −x; (ix) −x, −y, z; (x) z, −x, −y; (xi) −y, z, −x; (xii) x−1, y−1/2, z−1/2; (xiii) x, y−1/2, z−1/2; (xiv) x, y+1/2, z−1/2; (xv) z−1, x−1/2, y−1/2; (xvi) z, x−1/2, y−1/2; (xvii) z, x+1/2, y−1/2; (xviii) y−1, z−1/2, x−1/2; (xix) y, z−1/2, x−1/2; (xx) y, z+1/2, x−1/2; (xxi) x−1, y−1/2, −z−1/2; (xxii) x, y−1/2, −z−1/2; (xxiii) x, y+1/2, −z−1/2; (xxiv) −z−1, x−1/2, y−1/2; (xxv) −z, x−1/2, y−1/2; (xxvi) −z, x+1/2, y−1/2; (xxvii) y−1, −z−1/2, x−1/2; (xxviii) y, −z−1/2, x−1/2; (xxix) y, −z+1/2, x−1/2; (xxx) −x−1/2, −y−1, −z+1/2; (xxxi) −x−1/2, −y, −z+1/2; (xxxii) −x+1/2, −y, −z+1/2; (xxxiii) −z−1/2, −x−1, −y+1/2; (xxxiv) −z−1/2, −x, −y+1/2; (xxxv) −z+1/2, −x, −y+1/2; (xxxvi) −y−1/2, −z−1, −x+1/2; (xxxvii) −y−1/2, −z, −x+1/2; (xxxviii) −y+1/2, −z, −x+1/2; (xxxix) −x−1/2, −y−1, z+1/2; (xl) −x−1/2, −y, z+1/2; (xli) −x+1/2, −y, z+1/2; (xlii) z−1/2, −x−1, −y+1/2; (xliii) z−1/2, −x, −y+1/2; (xliv) z+1/2, −x, −y+1/2; (xlv) −y−1/2, z−1, −x+1/2; (xlvi) −y−1/2, z, −x+1/2; (xlvii) −y+1/2, z, −x+1/2; (xlviii) x−1/2, y−1, z+1/2; (xlix) x−1/2, y, z+1/2; (l) x+1/2, y, z+1/2; (li) −x−1, −y−1/2, −z+1/2; (lii) −x, −y−1/2, −z+1/2; (liii) −x, −y+1/2, −z+1/2; (liv) −z−1, −x−1/2, −y+1/2; (lv) −z, −x−1/2, −y+1/2; (lvi) −z, −x+1/2, −y+1/2; (lvii) −y−1, −z−1/2, −x+1/2; (lviii) −y, −z−1/2, −x+1/2; (lix) −y, −z+1/2, −x+1/2; (lx) −x, −y−1/2, z+1/2; (lxi) −x, −y+1/2, z+1/2; (lxii) z−1, −x−1/2, −y+1/2; (lxiii) z, −x+1/2, −y+1/2; (lxiv) −y−1, z−1/2, −x+1/2; (lxv) −y, z−1/2, −x+1/2; (lxvi) −x−1, −y−1/2, z+1/2; (lxvii) z, −x−1/2, −y+1/2; (lxviii) −y, z+1/2, −x+1/2; (lxix) z−1/2, x, y+1/2; (lxx) z+1/2, x, y+1/2; (lxxi) y−1/2, z−1, x+1/2; (lxxii) y−1/2, z, x+1/2; (lxxiii) x−1/2, y−1, −z+1/2; (lxxiv) x−1/2, y, −z+1/2; (lxxv) −z−1/2, x−1, y+1/2; (lxxvi) −z+1/2, x, y+1/2; (lxxvii) y−1/2, −z, x+1/2; (lxxviii) y+1/2, −z, x+1/2; (lxxix) −x, −y, −z+1; (lxxx) x, y−1, z; (lxxxi) x+1, y, z; (lxxxii) z, x+1, y; (lxxxiii) z+1, x+1, y; (lxxxiv) y−1, z−1, x; (lxxxv) y−1, z, x; (lxxxvi) x−1, y−1, −z; (lxxxvii) x−1, y, −z; (lxxxviii) −z, x−1, y; (lxxxix) −z+1, x, y; (xc) y, −z+1, x; (xci) y+1, −z+1, x; (xcii) −z, −x, −y+1; (xciii) −y, −z, −x+1; (xciv) −x, −y, z+1; (xcv) z, −x, −y+1; (xcvi) −y, z, −x+1; (xcvii) −z−1/2, x, y+1/2; (xcviii) x−1, y, z; (xcix) x, y+1, z; (100) −x, −y+1, −z+1; (101) z−1, −x, −y+1; (102) z, −x+1, −y+1.

(S3P1_phase_1)

Crystal data

O8P2Pb3	V = 724.65 (10) Å^3
Mr = 811.74	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.8108 (14) Å	T = 298 K
b = 5.6952 (7) Å	Particle morphology: plate
c = 9.4315 (9) Å	irregular, 6 × 6 mm
β = 102.358 (10)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.474 < d < 2.540 Angstrom (contamination from unidentified phase), 2.911 < d < 3.020 Angstrom (contamination from unidentified phase), d > 3.733 Angstrom (no useful data)
Rp = 0.054	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 51.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.09 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 140.2 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 401.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.041	50 parameters
Rexp = 0.034	10 restraints
R(F^2) = 0.20626	(Δ/σ)max = 0.01
χ^2 = 1.488	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.38467 2: -0.258231 3: 0.499498 4: -3.244690E-02 5: 0.134063 6: -4.495100E-03 7: 3.430580E-02 8: 1.433170E-02 9: 2.251290E-0210: -1.621240E-0211: 1.881670E-0212: 1.637730E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.86161 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.0	0.284 (3)	0.25	0.024 (2)*
Pb2	0.3169 (6)	0.3092 (16)	0.3492 (10)	0.024 (2)*
P	0.6013 (4)	0.2523 (15)	0.4476 (7)	0.027 (4)*
O21	0.6460 (8)	0.029 (2)	0.3903 (14)	0.016 (2)*
O22	0.6290 (8)	0.469 (2)	0.3697 (12)	0.016 (2)*
O23	0.6428 (8)	0.277 (2)	0.6119 (10)	0.016 (2)*
O1	0.4903 (6)	0.230 (2)	0.4191 (13)	0.016 (2)*

Geometric parameters (Å, º)

Pb1—Pb2	4.277 (8)	O21—Pb2^x	2.898 (17)
Pb1—Pb2^i	4.277 (8)	O21—Pb2^xi	3.079 (16)
Pb1—Pb2^ii	3.947 (14)	O21—Pb2^xii	4.466 (13)
Pb1—Pb2^iii	4.153 (15)	O21—Pb2^viii	2.773 (13)
Pb1—Pb2^iv	3.947 (14)	O21—P	1.557 (10)
Pb1—Pb2^v	4.153 (15)	O21—P^x	4.333 (16)
Pb1—Pb2^vi	4.108 (8)	O21—P^xi	4.337 (15)
Pb1—Pb2^vii	4.108 (8)	O21—P^xvii	4.392 (11)
Pb1—P^ii	3.670 (14)	O21—P^xiv	3.712 (15)
Pb1—P^iii	3.383 (13)	O21—O21^x	4.32 (2)
Pb1—P^iv	3.670 (14)	O21—O21^xix	4.49 (2)
Pb1—P^v	3.383 (13)	O21—O21^xiv	4.04 (2)
Pb1—P^vi	3.442 (6)	O21—O22^xx	3.204 (12)
Pb1—P^vii	3.442 (6)	O21—O22	2.517 (11)
Pb1—O21^iii	2.576 (14)	O21—O22^xxi	4.365 (11)
Pb1—O21^v	2.576 (14)	O21—O22^xiv	3.430 (17)
Pb1—O21^vi	4.431 (11)	O21—O23	2.529 (11)
Pb1—O21^vii	4.431 (11)	O21—O23^xi	4.349 (15)
Pb1—O22^ii	2.608 (16)	O21—O23^xvii	3.146 (16)
Pb1—O22^iii	4.339 (18)	O21—O23^xiv	3.123 (15)
Pb1—O22^iv	2.608 (16)	O21—O1	2.500 (11)
Pb1—O22^v	4.339 (18)	O21—O1^x	3.319 (15)
Pb1—O23^vi	2.608 (12)	O21—O1^xi	3.225 (16)
Pb1—O23^vii	2.608 (12)	O22—Pb1^viii	4.339 (18)
Pb1—O1^ii	3.548 (17)	O22—Pb1^ix	2.608 (16)
Pb1—O1^iii	3.020 (17)	O22—Pb2	4.370 (12)
Pb1—O1^iv	3.548 (17)	O22—Pb2^x	2.511 (15)
Pb1—O1^v	3.020 (17)	O22—Pb2^xii	2.887 (15)
Pb1—O1^vi	3.096 (12)	O22—Pb2^ix	3.277 (11)
Pb1—O1^vii	3.096 (12)	O22—P	1.525 (10)
Pb2—Pb1	4.277 (8)	O22—P^x	4.065 (14)
Pb2—Pb1^viii	4.153 (15)	O22—P^xii	4.238 (16)
Pb2—Pb1^ix	3.947 (14)	O22—P^xviii	4.227 (10)
Pb2—Pb1^vi	4.108 (8)	O22—P^xiv	3.959 (15)
Pb2—Pb2^iv	3.679 (10)	O22—O21	2.517 (11)
Pb2—Pb2^v	3.679 (10)	O22—O21^xxii	3.204 (12)
Pb2—Pb2^vi	3.77 (2)	O22—O21^xxiii	4.365 (11)
Pb2—P	3.853 (10)	O22—O21^xiv	3.430 (17)
Pb2—P^x	3.251 (12)	O22—O22^x	3.79 (2)
Pb2—P^xi	3.775 (12)	O22—O22^xiv	4.46 (2)
Pb2—P^xii	3.203 (12)	O22—O23	2.502 (11)
Pb2—P^iii	4.156 (12)	O22—O23^xii	4.062 (17)
Pb2—P^vii	4.301 (11)	O22—O23^xviii	2.871 (16)
Pb2—O21^x	2.898 (17)	O22—O23^xiv	3.418 (17)
Pb2—O21^xi	3.079 (16)	O22—O1	2.474 (11)
Pb2—O21^xii	4.466 (13)	O22—O1^x	3.173 (14)
Pb2—O21^iii	2.773 (13)	O22—O1^xii	3.321 (17)
Pb2—O22	4.370 (12)	O23—Pb1^vi	2.608 (12)
Pb2—O22^x	2.511 (15)	O23—Pb2^xi	3.392 (15)
Pb2—O22^xii	2.887 (15)	O23—Pb2^xii	2.431 (15)
Pb2—O22^ii	3.277 (11)	O23—Pb2^xiii	2.953 (11)
Pb2—O23^xi	3.392 (15)	O23—P	1.540 (9)
Pb2—O23^xii	2.431 (15)	O23—P^xi	4.468 (16)
Pb2—O23^vii	2.953 (11)	O23—P^xii	4.249 (17)
Pb2—O1	2.388 (12)	O23—P^xv	4.496 (14)
Pb2—O1^x	4.072 (14)	O23—P^xvi	4.279 (15)
Pb2—O1^xi	4.337 (14)	O23—P^xiv	3.698 (15)
Pb2—O1^xii	4.033 (15)	O23—O21	2.529 (11)
P—Pb1^viii	3.383 (13)	O23—O21^xi	4.349 (15)
P—Pb1^ix	3.670 (14)	O23—O21^xv	3.146 (16)
P—Pb1^vi	3.442 (6)	O23—O21^xiv	3.123 (15)
P—Pb2	3.853 (10)	O23—O22	2.502 (11)
P—Pb2^x	3.251 (12)	O23—O22^xii	4.062 (17)
P—Pb2^xi	3.775 (12)	O23—O22^xvi	2.871 (16)
P—Pb2^xii	3.203 (12)	O23—O22^xiv	3.418 (17)
P—Pb2^viii	4.156 (12)	O23—O23^xiv	4.00 (2)
P—Pb2^xiii	4.301 (11)	O23—O1	2.485 (10)
P—P^x	4.155 (13)	O23—O1^xi	3.402 (18)
P—P^xi	4.273 (14)	O23—O1^xii	3.334 (18)
P—P^xii	4.237 (14)	O1—Pb1^viii	3.020 (17)
P—P^xiv	4.013 (10)	O1—Pb1^ix	3.548 (17)
P—O21	1.557 (10)	O1—Pb1^vi	3.096 (12)
P—O21^x	4.333 (16)	O1—Pb2	2.388 (12)
P—O21^xi	4.337 (15)	O1—Pb2^x	4.072 (14)
P—O21^xv	4.392 (11)	O1—Pb2^xi	4.337 (14)
P—O21^xiv	3.712 (15)	O1—Pb2^xii	4.033 (15)
P—O22	1.525 (10)	O1—P	1.504 (8)
P—O22^x	4.065 (14)	O1—P^x	3.421 (16)
P—O22^xii	4.238 (16)	O1—P^xi	3.378 (17)
P—O22^xvi	4.227 (10)	O1—P^xii	3.543 (17)
P—O22^xiv	3.959 (15)	O1—O21	2.500 (11)
P—O23	1.540 (9)	O1—O21^x	3.319 (15)
P—O23^xi	4.468 (16)	O1—O21^xi	3.225 (16)
P—O23^xii	4.249 (17)	O1—O22	2.474 (11)
P—O23^xvii	4.496 (14)	O1—O22^x	3.173 (14)
P—O23^xviii	4.279 (15)	O1—O22^xii	3.321 (17)
P—O23^xiv	3.698 (15)	O1—O23	2.485 (10)
P—O1	1.504 (8)	O1—O23^xi	3.402 (18)
P—O1^x	3.421 (16)	O1—O23^xii	3.334 (18)
P—O1^xi	3.378 (17)	O1—O1^x	3.26 (2)
P—O1^xii	3.543 (17)	O1—O1^xi	3.02 (2)
O21—Pb1^viii	2.576 (14)	O1—O1^xii	3.42 (2)
O21—Pb1^vi	4.431 (11)
O21—P—O22	109.48 (14)	O22—P—O23	109.45 (13)
O21—P—O23	109.52 (13)	O22—P—O1	109.49 (13)
O21—P—O1	109.46 (14)	O23—P—O1	109.43 (15)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, −y, z+3/2; (xvi) x, −y+1, z+3/2; (xvii) x, −y, z+1/2; (xviii) x, −y+1, z+1/2; (xix) −x+3/2, −y−1/2, −z+1; (xx) x, y−1, z; (xxi) −x+3/2, y−1/2, −z+1/2; (xxii) x, y+1, z; (xxiii) −x+3/2, y+1/2, −z+1/2.

(S3P1_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.9017 (9) Å	T = 298 K
c = 2.8339 (14) Å	Particle morphology: Pressure cell anvil material
V = 20.66 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.474 < d < 2.540 Angstrom (contamination from unidentified phase), 2.911 < d < 3.020 Angstrom (contamination from unidentified phase), d > 3.733 Angstrom (no useful data)
Rp = 0.054	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 51.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.09 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 140.2 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 401.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.041	50 parameters
Rexp = 0.034	10 restraints
R(F^2) = 0.20626	(Δ/σ)max = 0.01
χ^2 = 1.488	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.38467 2: -0.258231 3: 0.499498 4: -3.244690E-02 5: 0.134063 6: -4.495100E-03 7: 3.430580E-02 8: 1.433170E-02 9: 2.251290E-0210: -1.621240E-0211: 1.881670E-0212: 1.637730E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.86161 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W(1)	0.0	0.0	0.0	0.025*
C(2)	0.66667	0.33333	0.5	0.025*

(S3P1_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5439 (11) Å	Particle morphology: Component of pressure cell, not sample
V = 44.51 (5) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.474 < d < 2.540 Angstrom (contamination from unidentified phase), 2.911 < d < 3.020 Angstrom (contamination from unidentified phase), d > 3.733 Angstrom (no useful data)
Rp = 0.054	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 51.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.09 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 140.2 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 401.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.041	50 parameters
Rexp = 0.034	10 restraints
R(F^2) = 0.20626	(Δ/σ)max = 0.01
χ^2 = 1.488	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.38467 2: -0.258231 3: 0.499498 4: -3.244690E-02 5: 0.134063 6: -4.495100E-03 7: 3.430580E-02 8: 1.433170E-02 9: 2.251290E-0210: -1.621240E-0211: 1.881670E-0212: 1.637730E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.86161 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.277 (8)	O21—Pb2^x	2.898 (17)
Pb1—Pb2^i	4.277 (8)	O21—Pb2^xi	3.079 (16)
Pb1—Pb2^ii	3.947 (14)	O21—Pb2^xii	4.466 (13)
Pb1—Pb2^iii	4.153 (15)	O21—Pb2^viii	2.773 (13)
Pb1—Pb2^iv	3.947 (14)	O21—P	1.557 (10)
Pb1—Pb2^v	4.153 (15)	O21—P^x	4.333 (16)
Pb1—Pb2^vi	4.108 (8)	O21—P^xi	4.337 (15)
Pb1—Pb2^vii	4.108 (8)	O21—P^xvii	4.392 (11)
Pb1—P^ii	3.670 (14)	O21—P^xiv	3.712 (15)
Pb1—P^iii	3.383 (13)	O21—O21^x	4.32 (2)
Pb1—P^iv	3.670 (14)	O21—O21^xix	4.49 (2)
Pb1—P^v	3.383 (13)	O21—O21^xiv	4.04 (2)
Pb1—P^vi	3.442 (6)	O21—O22^xx	3.204 (12)
Pb1—P^vii	3.442 (6)	O21—O22	2.517 (11)
Pb1—O21^iii	2.576 (14)	O21—O22^xxi	4.365 (11)
Pb1—O21^v	2.576 (14)	O21—O22^xiv	3.430 (17)
Pb1—O21^vi	4.431 (11)	O21—O23	2.529 (11)
Pb1—O21^vii	4.431 (11)	O21—O23^xi	4.349 (15)
Pb1—O22^ii	2.608 (16)	O21—O23^xvii	3.146 (16)
Pb1—O22^iii	4.339 (18)	O21—O23^xiv	3.123 (15)
Pb1—O22^iv	2.608 (16)	O21—O1	2.500 (11)
Pb1—O22^v	4.339 (18)	O21—O1^x	3.319 (15)
Pb1—O23^vi	2.608 (12)	O21—O1^xi	3.225 (16)
Pb1—O23^vii	2.608 (12)	O22—Pb1^viii	4.339 (18)
Pb1—O1^ii	3.548 (17)	O22—Pb1^ix	2.608 (16)
Pb1—O1^iii	3.020 (17)	O22—Pb2	4.370 (12)
Pb1—O1^iv	3.548 (17)	O22—Pb2^x	2.511 (15)
Pb1—O1^v	3.020 (17)	O22—Pb2^xii	2.887 (15)
Pb1—O1^vi	3.096 (12)	O22—Pb2^ix	3.277 (11)
Pb1—O1^vii	3.096 (12)	O22—P	1.525 (10)
Pb2—Pb1	4.277 (8)	O22—P^x	4.065 (14)
Pb2—Pb1^viii	4.153 (15)	O22—P^xii	4.238 (16)
Pb2—Pb1^ix	3.947 (14)	O22—P^xviii	4.227 (10)
Pb2—Pb1^vi	4.108 (8)	O22—P^xiv	3.959 (15)
Pb2—Pb2^iv	3.679 (10)	O22—O21	2.517 (11)
Pb2—Pb2^v	3.679 (10)	O22—O21^xxii	3.204 (12)
Pb2—Pb2^vi	3.77 (2)	O22—O21^xxiii	4.365 (11)
Pb2—P	3.853 (10)	O22—O21^xiv	3.430 (17)
Pb2—P^x	3.251 (12)	O22—O22^x	3.79 (2)
Pb2—P^xi	3.775 (12)	O22—O22^xiv	4.46 (2)
Pb2—P^xii	3.203 (12)	O22—O23	2.502 (11)
Pb2—P^iii	4.156 (12)	O22—O23^xii	4.062 (17)
Pb2—P^vii	4.301 (11)	O22—O23^xviii	2.871 (16)
Pb2—O21^x	2.898 (17)	O22—O23^xiv	3.418 (17)
Pb2—O21^xi	3.079 (16)	O22—O1	2.474 (11)
Pb2—O21^xii	4.466 (13)	O22—O1^x	3.173 (14)
Pb2—O21^iii	2.773 (13)	O22—O1^xii	3.321 (17)
Pb2—O22	4.370 (12)	O23—Pb1^vi	2.608 (12)
Pb2—O22^x	2.511 (15)	O23—Pb2^xi	3.392 (15)
Pb2—O22^xii	2.887 (15)	O23—Pb2^xii	2.431 (15)
Pb2—O22^ii	3.277 (11)	O23—Pb2^xiii	2.953 (11)
Pb2—O23^xi	3.392 (15)	O23—P	1.540 (9)
Pb2—O23^xii	2.431 (15)	O23—P^xi	4.468 (16)
Pb2—O23^vii	2.953 (11)	O23—P^xii	4.249 (17)
Pb2—O1	2.388 (12)	O23—P^xv	4.496 (14)
Pb2—O1^x	4.072 (14)	O23—P^xvi	4.279 (15)
Pb2—O1^xi	4.337 (14)	O23—P^xiv	3.698 (15)
Pb2—O1^xii	4.033 (15)	O23—O21	2.529 (11)
P—Pb1^viii	3.383 (13)	O23—O21^xi	4.349 (15)
P—Pb1^ix	3.670 (14)	O23—O21^xv	3.146 (16)
P—Pb1^vi	3.442 (6)	O23—O21^xiv	3.123 (15)
P—Pb2	3.853 (10)	O23—O22	2.502 (11)
P—Pb2^x	3.251 (12)	O23—O22^xii	4.062 (17)
P—Pb2^xi	3.775 (12)	O23—O22^xvi	2.871 (16)
P—Pb2^xii	3.203 (12)	O23—O22^xiv	3.418 (17)
P—Pb2^viii	4.156 (12)	O23—O23^xiv	4.00 (2)
P—Pb2^xiii	4.301 (11)	O23—O1	2.485 (10)
P—P^x	4.155 (13)	O23—O1^xi	3.402 (18)
P—P^xi	4.273 (14)	O23—O1^xii	3.334 (18)
P—P^xii	4.237 (14)	O1—Pb1^viii	3.020 (17)
P—P^xiv	4.013 (10)	O1—Pb1^ix	3.548 (17)
P—O21	1.557 (10)	O1—Pb1^vi	3.096 (12)
P—O21^x	4.333 (16)	O1—Pb2	2.388 (12)
P—O21^xi	4.337 (15)	O1—Pb2^x	4.072 (14)
P—O21^xv	4.392 (11)	O1—Pb2^xi	4.337 (14)
P—O21^xiv	3.712 (15)	O1—Pb2^xii	4.033 (15)
P—O22	1.525 (10)	O1—P	1.504 (8)
P—O22^x	4.065 (14)	O1—P^x	3.421 (16)
P—O22^xii	4.238 (16)	O1—P^xi	3.378 (17)
P—O22^xvi	4.227 (10)	O1—P^xii	3.543 (17)
P—O22^xiv	3.959 (15)	O1—O21	2.500 (11)
P—O23	1.540 (9)	O1—O21^x	3.319 (15)
P—O23^xi	4.468 (16)	O1—O21^xi	3.225 (16)
P—O23^xii	4.249 (17)	O1—O22	2.474 (11)
P—O23^xvii	4.496 (14)	O1—O22^x	3.173 (14)
P—O23^xviii	4.279 (15)	O1—O22^xii	3.321 (17)
P—O23^xiv	3.698 (15)	O1—O23	2.485 (10)
P—O1	1.504 (8)	O1—O23^xi	3.402 (18)
P—O1^x	3.421 (16)	O1—O23^xii	3.334 (18)
P—O1^xi	3.378 (17)	O1—O1^x	3.26 (2)
P—O1^xii	3.543 (17)	O1—O1^xi	3.02 (2)
O21—Pb1^viii	2.576 (14)	O1—O1^xii	3.42 (2)
O21—Pb1^vi	4.431 (11)
O21—P—O22	109.48 (14)	O22—P—O23	109.45 (13)
O21—P—O23	109.52 (13)	O22—P—O1	109.49 (13)
O21—P—O1	109.46 (14)	O23—P—O1	109.43 (15)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) −z, −x, −y+1; (xvi) −z, −x+1, −y+1; (xvii) −z, −x, −y; (xviii) −z, −x+1, −y; (xix) −x+1, −y−1/2, −z+3/2; (xx) x, y−1, z; (xxi) z+1, x−1/2, y+1/2; (xxii) x, y+1, z; (xxiii) z+1, x+1/2, y+1/2.

(S3P2_phase_1)

Crystal data

O8P2Pb3	V = 706.80 (12) Å^3
Mr = 811.74	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7849 (18) Å	T = 298 K
b = 5.5692 (7) Å	Particle morphology: plate
c = 9.4445 (10) Å	irregular, 6 × 6 mm
β = 102.887 (16)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.880 < d < 3.020 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.064	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 69.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 3.60 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 118.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 266.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.047	50 parameters
Rexp = 0.041	10 restraints
R(F^2) = 0.24302	(Δ/σ)max = 0.05
χ^2 = 1.346	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.13214 2: -0.352279 3: 0.447414 4: -0.128935 5: 0.128777 6: -9.664080E-02 7: 6.491590E-02 8: -7.468470E-02 9: 5.118870E-0210: -5.954540E-0211: 3.043490E-0212: -2.018070E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00666 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.0	0.274 (4)	0.25	0.040 (3)*
Pb2	0.3120 (6)	0.297 (2)	0.3512 (15)	0.040 (3)*
P	0.6032 (4)	0.2626 (18)	0.4522 (9)	0.024 (3)*
O21	0.6448 (11)	0.026 (3)	0.4024 (15)	0.018 (2)*
O22	0.6434 (11)	0.476 (3)	0.3813 (15)	0.018 (2)*
O23	0.6355 (9)	0.285 (2)	0.6171 (12)	0.018 (2)*
O1	0.4912 (6)	0.260 (3)	0.4076 (16)	0.018 (2)*

Geometric parameters (Å, º)

Pb1—Pb2	4.194 (9)	O21—Pb1^vi	4.351 (14)
Pb1—Pb2^i	4.194 (9)	O21—Pb2^x	3.00 (2)
Pb1—Pb2^ii	3.97 (2)	O21—Pb2^xi	2.90 (2)
Pb1—Pb2^iii	4.15 (2)	O21—Pb2^xii	4.403 (17)
Pb1—Pb2^iv	3.97 (2)	O21—Pb2^viii	2.768 (17)
Pb1—Pb2^v	4.15 (2)	O21—Pb2^xiii	4.460 (18)
Pb1—Pb2^vi	4.088 (12)	O21—P^xvii	4.327 (11)
Pb1—Pb2^vii	4.088 (12)	O21—P	1.553 (10)
Pb1—P^ii	3.55 (2)	O21—P^x	4.420 (18)
Pb1—P^iii	3.44 (2)	O21—P^xi	4.27 (2)
Pb1—P^iv	3.55 (2)	O21—P^xix	4.460 (11)
Pb1—P^v	3.44 (2)	O21—P^xiv	3.635 (19)
Pb1—P^vi	3.430 (8)	O21—O21^x	4.37 (3)
Pb1—P^vii	3.430 (8)	O21—O21^xxi	4.34 (3)
Pb1—O21^iii	2.60 (2)	O21—O21^xiv	3.96 (3)
Pb1—O21^v	2.60 (2)	O21—O22^xvii	3.067 (11)
Pb1—O21^vi	4.351 (14)	O21—O22	2.516 (11)
Pb1—O21^vii	4.351 (14)	O21—O22^xxii	4.388 (14)
Pb1—O22^ii	2.67 (2)	O21—O22^xiv	3.168 (18)
Pb1—O22^iii	4.43 (3)	O21—O23	2.515 (11)
Pb1—O22^iv	2.67 (2)	O21—O23^xi	4.20 (2)
Pb1—O22^v	4.43 (3)	O21—O23^xix	3.180 (18)
Pb1—O23^ii	4.478 (19)	O21—O23^xiv	3.25 (2)
Pb1—O23^iv	4.478 (19)	O21—O1	2.499 (11)
Pb1—O23^vi	2.494 (14)	O21—O1^x	3.369 (15)
Pb1—O23^vii	2.494 (14)	O21—O1^xi	3.28 (2)
Pb1—O1^ii	3.24 (3)	O22—Pb1^viii	4.43 (3)
Pb1—O1^iii	3.11 (3)	O22—Pb1^ix	2.67 (2)
Pb1—O1^iv	3.24 (3)	O22—Pb2^x	2.61 (2)
Pb1—O1^v	3.11 (3)	O22—Pb2^xii	2.77 (2)
Pb1—O1^vi	3.214 (15)	O22—Pb2^viii	4.48 (2)
Pb1—O1^vii	3.214 (15)	O22—Pb2^ix	2.995 (15)
Pb2—Pb1	4.194 (9)	O22—P	1.528 (10)
Pb2—Pb1^viii	4.15 (2)	O22—P^xv	4.484 (13)
Pb2—Pb1^ix	3.97 (2)	O22—P^x	4.256 (18)
Pb2—Pb1^vi	4.088 (12)	O22—P^xii	4.31 (2)
Pb2—Pb2^iv	3.587 (14)	O22—P^xx	4.224 (11)
Pb2—Pb2^v	3.587 (14)	O22—P^xiv	3.74 (2)
Pb2—Pb2^vi	3.64 (3)	O22—O21	2.516 (11)
Pb2—P	3.919 (11)	O22—O21^xv	3.067 (11)
Pb2—P^x	3.333 (18)	O22—O21^xxiii	4.388 (14)
Pb2—P^xi	3.683 (15)	O22—O21^xiv	3.168 (18)
Pb2—P^xii	3.140 (16)	O22—O22^x	4.17 (3)
Pb2—P^ii	4.390 (14)	O22—O22^xiv	4.13 (3)
Pb2—P^iii	4.140 (15)	O22—O22^xxiv	4.48 (3)
Pb2—P^vii	4.214 (13)	O22—O23	2.493 (11)
Pb2—O21^x	3.00 (2)	O22—O23^xii	4.07 (2)
Pb2—O21^xi	2.90 (2)	O22—O23^xx	2.809 (15)
Pb2—O21^xii	4.403 (17)	O22—O23^xiv	3.37 (2)
Pb2—O21^iii	2.768 (17)	O22—O1	2.478 (11)
Pb2—O21^vii	4.460 (18)	O22—O1^x	3.174 (16)
Pb2—O22^x	2.61 (2)	O22—O1^xii	3.35 (2)
Pb2—O22^xii	2.77 (2)	O23—Pb1^ix	4.478 (19)
Pb2—O22^ii	2.995 (15)	O23—Pb1^vi	2.494 (14)
Pb2—O22^iii	4.48 (2)	O23—Pb2^xi	3.319 (16)
Pb2—O23^xi	3.319 (16)	O23—Pb2^xii	2.438 (16)
Pb2—O23^xii	2.438 (16)	O23—Pb2^xiii	2.935 (13)
Pb2—O23^vii	2.935 (13)	O23—P	1.526 (10)
Pb2—O1	2.417 (12)	O23—P^xi	4.426 (19)
Pb2—O1^x	4.041 (19)	O23—P^xii	4.081 (17)
Pb2—O1^xi	4.408 (19)	O23—P^xvi	4.487 (17)
Pb2—O1^xii	3.983 (18)	O23—P^xviii	4.148 (14)
P—Pb1^viii	3.44 (2)	O23—P^xiv	3.811 (16)
P—Pb1^ix	3.55 (2)	O23—O21	2.515 (11)
P—Pb1^vi	3.430 (8)	O23—O21^xi	4.20 (2)
P—Pb2	3.919 (11)	O23—O21^xvi	3.180 (18)
P—Pb2^x	3.333 (18)	O23—O21^xiv	3.25 (2)
P—Pb2^xi	3.683 (15)	O23—O22	2.493 (11)
P—Pb2^xii	3.140 (16)	O23—O22^xii	4.07 (2)
P—Pb2^viii	4.140 (15)	O23—O22^xviii	2.809 (15)
P—Pb2^ix	4.390 (14)	O23—O22^xiv	3.37 (2)
P—Pb2^xiii	4.214 (13)	O23—O23^xiv	4.26 (3)
P—P^x	4.223 (14)	O23—O1	2.476 (10)
P—P^xi	4.315 (16)	O23—O1^xi	3.48 (2)
P—P^xii	4.129 (16)	O23—O1^xii	3.057 (19)
P—P^xiv	3.948 (10)	O1—Pb1^viii	3.11 (3)
P—O21	1.553 (10)	O1—Pb1^ix	3.24 (3)
P—O21^xv	4.327 (11)	O1—Pb1^vi	3.214 (15)
P—O21^x	4.420 (18)	O1—Pb2	2.417 (12)
P—O21^xi	4.27 (2)	O1—Pb2^x	4.041 (19)
P—O21^xvi	4.460 (11)	O1—Pb2^xi	4.408 (19)
P—O21^xiv	3.635 (19)	O1—Pb2^xii	3.983 (18)
P—O22^xvii	4.484 (13)	O1—P	1.507 (8)
P—O22	1.528 (10)	O1—P^x	3.357 (19)
P—O22^x	4.256 (18)	O1—P^xi	3.56 (2)
P—O22^xii	4.31 (2)	O1—P^xii	3.36 (2)
P—O22^xviii	4.224 (11)	O1—O21	2.499 (11)
P—O22^xiv	3.74 (2)	O1—O21^x	3.369 (15)
P—O23	1.526 (10)	O1—O21^xi	3.28 (2)
P—O23^xi	4.426 (19)	O1—O22	2.478 (11)
P—O23^xii	4.081 (17)	O1—O22^x	3.174 (16)
P—O23^xix	4.487 (17)	O1—O22^xii	3.35 (2)
P—O23^xx	4.148 (14)	O1—O23	2.476 (10)
P—O23^xiv	3.811 (16)	O1—O23^xi	3.48 (2)
P—O1	1.507 (8)	O1—O23^xii	3.057 (19)
P—O1^x	3.357 (19)	O1—O1^x	3.04 (3)
P—O1^xi	3.56 (2)	O1—O1^xi	3.37 (3)
P—O1^xii	3.36 (2)	O1—O1^xii	3.17 (3)
O21—Pb1^viii	2.60 (2)
O21—P—O22	109.49 (14)	O22—P—O23	109.45 (14)
O21—P—O23	109.51 (14)	O22—P—O1	109.47 (14)
O21—P—O1	109.46 (14)	O23—P—O1	109.46 (15)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, y−1, z; (xviii) x, −y+1, z+3/2; (xix) x, −y, z+1/2; (xx) x, −y+1, z+1/2; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2; (xxiv) −x+3/2, −y+3/2, −z+1.

(S3P2_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.9030 (9) Å	T = 298 K
c = 2.8315 (14) Å	Particle morphology: Pressure cell anvil material
V = 20.67 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.880 < d < 3.020 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.064	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 69.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 3.60 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 118.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 266.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.047	50 parameters
Rexp = 0.041	10 restraints
R(F^2) = 0.24302	(Δ/σ)max = 0.05
χ^2 = 1.346	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.13214 2: -0.352279 3: 0.447414 4: -0.128935 5: 0.128777 6: -9.664080E-02 7: 6.491590E-02 8: -7.468470E-02 9: 5.118870E-0210: -5.954540E-0211: 3.043490E-0212: -2.018070E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00666 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W(1)	0.0	0.0	0.0	0.025*
C(2)	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.194 (9)	O21—Pb1	4.351 (14)
Pb1—Pb2^i	4.194 (9)	O21—Pb2^ii	3.00 (2)
Pb1—Pb2	3.97 (2)	O21—Pb2	2.90 (2)
Pb1—Pb2	4.15 (2)	O21—Pb2	4.403 (17)
Pb1—Pb2	3.97 (2)	O21—Pb2	2.768 (17)
Pb1—Pb2	4.15 (2)	O21—Pb2	4.460 (18)
Pb1—Pb2	4.088 (12)	O21—P^iv	4.327 (11)
Pb1—Pb2	4.088 (12)	O21—P	1.553 (10)
Pb1—P	3.55 (2)	O21—P^ii	4.420 (18)
Pb1—P	3.44 (2)	O21—P	4.27 (2)
Pb1—P	3.55 (2)	O21—P	4.460 (11)
Pb1—P	3.44 (2)	O21—P	3.635 (19)
Pb1—P	3.430 (8)	O21—O21^ii	4.37 (3)
Pb1—P	3.430 (8)	O21—O21	4.34 (3)
Pb1—O21	2.60 (2)	O21—O21	3.96 (3)
Pb1—O21	2.60 (2)	O21—O22^iv	3.067 (11)
Pb1—O21	4.351 (14)	O21—O22	2.516 (11)
Pb1—O21	4.351 (14)	O21—O22	4.388 (14)
Pb1—O22	2.67 (2)	O21—O22	3.168 (18)
Pb1—O22	4.43 (3)	O21—O23	2.515 (11)
Pb1—O22	2.67 (2)	O21—O23	4.20 (2)
Pb1—O22	4.43 (3)	O21—O23	3.180 (18)
Pb1—O23	4.478 (19)	O21—O23	3.25 (2)
Pb1—O23	4.478 (19)	O21—O1	2.499 (11)
Pb1—O23	2.494 (14)	O21—O1^ii	3.369 (15)
Pb1—O23	2.494 (14)	O21—O1	3.28 (2)
Pb1—O1	3.24 (3)	O22—Pb1	4.43 (3)
Pb1—O1	3.11 (3)	O22—Pb1	2.67 (2)
Pb1—O1	3.24 (3)	O22—Pb2^ii	2.61 (2)
Pb1—O1	3.11 (3)	O22—Pb2	2.77 (2)
Pb1—O1	3.214 (15)	O22—Pb2	4.48 (2)
Pb1—O1	3.214 (15)	O22—Pb2	2.995 (15)
Pb2—Pb1	4.194 (9)	O22—P	1.528 (10)
Pb2—Pb1	4.15 (2)	O22—P^iii	4.484 (13)
Pb2—Pb1	3.97 (2)	O22—P^ii	4.256 (18)
Pb2—Pb1	4.088 (12)	O22—P	4.31 (2)
Pb2—Pb2	3.587 (14)	O22—P	4.224 (11)
Pb2—Pb2	3.587 (14)	O22—P	3.74 (2)
Pb2—Pb2	3.64 (3)	O22—O21	2.516 (11)
Pb2—P	3.919 (11)	O22—O21^iii	3.067 (11)
Pb2—P^ii	3.333 (18)	O22—O21	4.388 (14)
Pb2—P	3.683 (15)	O22—O21	3.168 (18)
Pb2—P	3.140 (16)	O22—O22^ii	4.17 (3)
Pb2—P	4.390 (14)	O22—O22	4.13 (3)
Pb2—P	4.140 (15)	O22—O22	4.48 (3)
Pb2—P	4.214 (13)	O22—O23	2.493 (11)
Pb2—O21^ii	3.00 (2)	O22—O23	4.07 (2)
Pb2—O21	2.90 (2)	O22—O23	2.809 (15)
Pb2—O21	4.403 (17)	O22—O23	3.37 (2)
Pb2—O21	2.768 (17)	O22—O1	2.478 (11)
Pb2—O21	4.460 (18)	O22—O1^ii	3.174 (16)
Pb2—O22^ii	2.61 (2)	O22—O1	3.35 (2)
Pb2—O22	2.77 (2)	O23—Pb1	4.478 (19)
Pb2—O22	2.995 (15)	O23—Pb1	2.494 (14)
Pb2—O22	4.48 (2)	O23—Pb2	3.319 (16)
Pb2—O23	3.319 (16)	O23—Pb2	2.438 (16)
Pb2—O23	2.438 (16)	O23—Pb2	2.935 (13)
Pb2—O23	2.935 (13)	O23—P	1.526 (10)
Pb2—O1	2.417 (12)	O23—P	4.426 (19)
Pb2—O1^ii	4.041 (19)	O23—P	4.081 (17)
Pb2—O1	4.408 (19)	O23—P	4.487 (17)
Pb2—O1	3.983 (18)	O23—P	4.148 (14)
P—Pb1	3.44 (2)	O23—P	3.811 (16)
P—Pb1	3.55 (2)	O23—O21	2.515 (11)
P—Pb1	3.430 (8)	O23—O21	4.20 (2)
P—Pb2	3.919 (11)	O23—O21	3.180 (18)
P—Pb2^ii	3.333 (18)	O23—O21	3.25 (2)
P—Pb2	3.683 (15)	O23—O22	2.493 (11)
P—Pb2	3.140 (16)	O23—O22	4.07 (2)
P—Pb2	4.140 (15)	O23—O22	2.809 (15)
P—Pb2	4.390 (14)	O23—O22	3.37 (2)
P—Pb2	4.214 (13)	O23—O23	4.26 (3)
P—P^ii	4.223 (14)	O23—O1	2.476 (10)
P—P	4.315 (16)	O23—O1	3.48 (2)
P—P	4.129 (16)	O23—O1	3.057 (19)
P—P	3.948 (10)	O1—Pb1	3.11 (3)
P—O21	1.553 (10)	O1—Pb1	3.24 (3)
P—O21^iii	4.327 (11)	O1—Pb1	3.214 (15)
P—O21^ii	4.420 (18)	O1—Pb2	2.417 (12)
P—O21	4.27 (2)	O1—Pb2^ii	4.041 (19)
P—O21	4.460 (11)	O1—Pb2	4.408 (19)
P—O21	3.635 (19)	O1—Pb2	3.983 (18)
P—O22^iv	4.484 (13)	O1—P	1.507 (8)
P—O22	1.528 (10)	O1—P^ii	3.357 (19)
P—O22^ii	4.256 (18)	O1—P	3.56 (2)
P—O22	4.31 (2)	O1—P	3.36 (2)
P—O22	4.224 (11)	O1—O21	2.499 (11)
P—O22	3.74 (2)	O1—O21^ii	3.369 (15)
P—O23	1.526 (10)	O1—O21	3.28 (2)
P—O23	4.426 (19)	O1—O22	2.478 (11)
P—O23	4.081 (17)	O1—O22^ii	3.174 (16)
P—O23	4.487 (17)	O1—O22	3.35 (2)
P—O23	4.148 (14)	O1—O23	2.476 (10)
P—O23	3.811 (16)	O1—O23	3.48 (2)
P—O1	1.507 (8)	O1—O23	3.057 (19)
P—O1^ii	3.357 (19)	O1—O1^ii	3.04 (3)
P—O1	3.56 (2)	O1—O1	3.37 (3)
P—O1	3.36 (2)	O1—O1	3.17 (3)
O21—Pb1	2.60 (2)
O21—P—O22	109.49 (14)	O22—P—O23	109.45 (14)
O21—P—O23	109.51 (14)	O22—P—O1	109.47 (14)
O21—P—O1	109.46 (14)	O23—P—O1	109.46 (15)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(S3P2_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5421 (11) Å	Particle morphology: Component of pressure cell, not sample
V = 44.44 (5) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.880 < d < 3.020 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.064	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 69.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 3.60 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 118.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 266.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.047	50 parameters
Rexp = 0.041	10 restraints
R(F^2) = 0.24302	(Δ/σ)max = 0.05
χ^2 = 1.346	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.13214 2: -0.352279 3: 0.447414 4: -0.128935 5: 0.128777 6: -9.664080E-02 7: 6.491590E-02 8: -7.468470E-02 9: 5.118870E-0210: -5.954540E-0211: 3.043490E-0212: -2.018070E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 1.00666 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.194 (9)	O21—Pb1^vi	4.351 (14)
Pb1—Pb2^i	4.194 (9)	O21—Pb2^x	3.00 (2)
Pb1—Pb2^ii	3.97 (2)	O21—Pb2^xi	2.90 (2)
Pb1—Pb2^iii	4.15 (2)	O21—Pb2^xii	4.403 (17)
Pb1—Pb2^iv	3.97 (2)	O21—Pb2^viii	2.768 (17)
Pb1—Pb2^v	4.15 (2)	O21—Pb2^xiii	4.460 (18)
Pb1—Pb2^vi	4.088 (12)	O21—P^xvii	4.327 (11)
Pb1—Pb2^vii	4.088 (12)	O21—P	1.553 (10)
Pb1—P^ii	3.55 (2)	O21—P^x	4.420 (18)
Pb1—P^iii	3.44 (2)	O21—P^xi	4.27 (2)
Pb1—P^iv	3.55 (2)	O21—P^xix	4.460 (11)
Pb1—P^v	3.44 (2)	O21—P^xiv	3.635 (19)
Pb1—P^vi	3.430 (8)	O21—O21^x	4.37 (3)
Pb1—P^vii	3.430 (8)	O21—O21^xxi	4.34 (3)
Pb1—O21^iii	2.60 (2)	O21—O21^xiv	3.96 (3)
Pb1—O21^v	2.60 (2)	O21—O22^xvii	3.067 (11)
Pb1—O21^vi	4.351 (14)	O21—O22	2.516 (11)
Pb1—O21^vii	4.351 (14)	O21—O22^xxii	4.388 (14)
Pb1—O22^ii	2.67 (2)	O21—O22^xiv	3.168 (18)
Pb1—O22^iii	4.43 (3)	O21—O23	2.515 (11)
Pb1—O22^iv	2.67 (2)	O21—O23^xi	4.20 (2)
Pb1—O22^v	4.43 (3)	O21—O23^xix	3.180 (18)
Pb1—O23^ii	4.478 (19)	O21—O23^xiv	3.25 (2)
Pb1—O23^iv	4.478 (19)	O21—O1	2.499 (11)
Pb1—O23^vi	2.494 (14)	O21—O1^x	3.369 (15)
Pb1—O23^vii	2.494 (14)	O21—O1^xi	3.28 (2)
Pb1—O1^ii	3.24 (3)	O22—Pb1^viii	4.43 (3)
Pb1—O1^iii	3.11 (3)	O22—Pb1^ix	2.67 (2)
Pb1—O1^iv	3.24 (3)	O22—Pb2^x	2.61 (2)
Pb1—O1^v	3.11 (3)	O22—Pb2^xii	2.77 (2)
Pb1—O1^vi	3.214 (15)	O22—Pb2^viii	4.48 (2)
Pb1—O1^vii	3.214 (15)	O22—Pb2^ix	2.995 (15)
Pb2—Pb1	4.194 (9)	O22—P	1.528 (10)
Pb2—Pb1^viii	4.15 (2)	O22—P^xv	4.484 (13)
Pb2—Pb1^ix	3.97 (2)	O22—P^x	4.256 (18)
Pb2—Pb1^vi	4.088 (12)	O22—P^xii	4.31 (2)
Pb2—Pb2^iv	3.587 (14)	O22—P^xx	4.224 (11)
Pb2—Pb2^v	3.587 (14)	O22—P^xiv	3.74 (2)
Pb2—Pb2^vi	3.64 (3)	O22—O21	2.516 (11)
Pb2—P	3.919 (11)	O22—O21^xv	3.067 (11)
Pb2—P^x	3.333 (18)	O22—O21^xxiii	4.388 (14)
Pb2—P^xi	3.683 (15)	O22—O21^xiv	3.168 (18)
Pb2—P^xii	3.140 (16)	O22—O22^x	4.17 (3)
Pb2—P^ii	4.390 (14)	O22—O22^xiv	4.13 (3)
Pb2—P^iii	4.140 (15)	O22—O22^xxiv	4.48 (3)
Pb2—P^vii	4.214 (13)	O22—O23	2.493 (11)
Pb2—O21^x	3.00 (2)	O22—O23^xii	4.07 (2)
Pb2—O21^xi	2.90 (2)	O22—O23^xx	2.809 (15)
Pb2—O21^xii	4.403 (17)	O22—O23^xiv	3.37 (2)
Pb2—O21^iii	2.768 (17)	O22—O1	2.478 (11)
Pb2—O21^vii	4.460 (18)	O22—O1^x	3.174 (16)
Pb2—O22^x	2.61 (2)	O22—O1^xii	3.35 (2)
Pb2—O22^xii	2.77 (2)	O23—Pb1^ix	4.478 (19)
Pb2—O22^ii	2.995 (15)	O23—Pb1^vi	2.494 (14)
Pb2—O22^iii	4.48 (2)	O23—Pb2^xi	3.319 (16)
Pb2—O23^xi	3.319 (16)	O23—Pb2^xii	2.438 (16)
Pb2—O23^xii	2.438 (16)	O23—Pb2^xiii	2.935 (13)
Pb2—O23^vii	2.935 (13)	O23—P	1.526 (10)
Pb2—O1	2.417 (12)	O23—P^xi	4.426 (19)
Pb2—O1^x	4.041 (19)	O23—P^xii	4.081 (17)
Pb2—O1^xi	4.408 (19)	O23—P^xvi	4.487 (17)
Pb2—O1^xii	3.983 (18)	O23—P^xviii	4.148 (14)
P—Pb1^viii	3.44 (2)	O23—P^xiv	3.811 (16)
P—Pb1^ix	3.55 (2)	O23—O21	2.515 (11)
P—Pb1^vi	3.430 (8)	O23—O21^xi	4.20 (2)
P—Pb2	3.919 (11)	O23—O21^xvi	3.180 (18)
P—Pb2^x	3.333 (18)	O23—O21^xiv	3.25 (2)
P—Pb2^xi	3.683 (15)	O23—O22	2.493 (11)
P—Pb2^xii	3.140 (16)	O23—O22^xii	4.07 (2)
P—Pb2^viii	4.140 (15)	O23—O22^xviii	2.809 (15)
P—Pb2^ix	4.390 (14)	O23—O22^xiv	3.37 (2)
P—Pb2^xiii	4.214 (13)	O23—O23^xiv	4.26 (3)
P—P^x	4.223 (14)	O23—O1	2.476 (10)
P—P^xi	4.315 (16)	O23—O1^xi	3.48 (2)
P—P^xii	4.129 (16)	O23—O1^xii	3.057 (19)
P—P^xiv	3.948 (10)	O1—Pb1^viii	3.11 (3)
P—O21	1.553 (10)	O1—Pb1^ix	3.24 (3)
P—O21^xv	4.327 (11)	O1—Pb1^vi	3.214 (15)
P—O21^x	4.420 (18)	O1—Pb2	2.417 (12)
P—O21^xi	4.27 (2)	O1—Pb2^x	4.041 (19)
P—O21^xvi	4.460 (11)	O1—Pb2^xi	4.408 (19)
P—O21^xiv	3.635 (19)	O1—Pb2^xii	3.983 (18)
P—O22^xvii	4.484 (13)	O1—P	1.507 (8)
P—O22	1.528 (10)	O1—P^x	3.357 (19)
P—O22^x	4.256 (18)	O1—P^xi	3.56 (2)
P—O22^xii	4.31 (2)	O1—P^xii	3.36 (2)
P—O22^xviii	4.224 (11)	O1—O21	2.499 (11)
P—O22^xiv	3.74 (2)	O1—O21^x	3.369 (15)
P—O23	1.526 (10)	O1—O21^xi	3.28 (2)
P—O23^xi	4.426 (19)	O1—O22	2.478 (11)
P—O23^xii	4.081 (17)	O1—O22^x	3.174 (16)
P—O23^xix	4.487 (17)	O1—O22^xii	3.35 (2)
P—O23^xx	4.148 (14)	O1—O23	2.476 (10)
P—O23^xiv	3.811 (16)	O1—O23^xi	3.48 (2)
P—O1	1.507 (8)	O1—O23^xii	3.057 (19)
P—O1^x	3.357 (19)	O1—O1^x	3.04 (3)
P—O1^xi	3.56 (2)	O1—O1^xi	3.37 (3)
P—O1^xii	3.36 (2)	O1—O1^xii	3.17 (3)
O21—Pb1^viii	2.60 (2)
O21—P—O22	109.49 (14)	O22—P—O23	109.45 (14)
O21—P—O23	109.51 (14)	O22—P—O1	109.47 (14)
O21—P—O1	109.46 (14)	O23—P—O1	109.46 (15)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) x, y+1, z; (xvi) −z, −x, −y+1; (xvii) x, y−1, z; (xviii) −z, −x+1, −y+1; (xix) −z, −x, −y; (xx) −z, −x+1, −y; (xxi) −x+1, −y−1/2, −z+3/2; (xxii) z+1, x−1/2, y+1/2; (xxiii) z+1, x+1/2, y+1/2; (xxiv) −x+1, −y+3/2, −z+3/2.

(S3P3X0_phase_1)

Crystal data

O8.00P2Pb3.00	Z = 3
Mr = 811.74	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.4552 (2) Å	Particle morphology: plate
c = 20.0656 (13) Å	irregular, 6 × 6 mm
V = 517.13 (4) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.880 < d < 2.995 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.042	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 71.4 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.80 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 96.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 118.2 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.034	36 parameters
Rexp = 0.025	0 restraints
R(F^2) = 0.18318	(Δ/σ)max < 0.001
χ^2 = 1.823	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.90809 2: -0.452429 3: 0.711020 4: -0.122874 5: 0.229419 6: -0.131639 7: 0.144616 8: -0.108729 9: 0.102496 10: -7.406590E-0211: 3.979930E-0212: -1.408490E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.84934 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pb1	0.0	0.0	0.0	0.0225 (18)*
Pb2	0.0	0.039 (2)	0.21001 (19)	0.0225 (18)*	0.16667
P	0.0	0.0	0.4038 (4)	0.0102 (15)*
O1	0.0	0.0	0.3283 (3)	0.0167 (12)*
O2	−0.137 (2)	0.172 (2)	0.42904 (16)	0.0167 (12)*	0.5

Geometric parameters (Å, º)

Pb1—Pb2	4.219 (4)	P—Pb2^xlviii	4.080 (10)
Pb1—Pb2^i	4.219 (4)	P—Pb2^xlix	4.356 (10)
Pb1—Pb2^ii	4.219 (4)	P—Pb2^l	4.220 (6)
Pb1—Pb2^iii	4.219 (4)	P—Pb2^lxix	4.356 (10)
Pb1—Pb2^iv	4.219 (4)	P—Pb2^lxx	4.220 (6)
Pb1—Pb2^v	4.219 (4)	P—Pb2^lxxi	4.080 (10)
Pb1—Pb2^vi	4.219 (4)	P—Pb2^lxxii	4.220 (6)
Pb1—Pb2^vii	4.219 (4)	P—Pb2^lxxiii	4.080 (10)
Pb1—Pb2^viii	4.219 (4)	P—Pb2^lxxiv	4.356 (10)
Pb1—Pb2^ix	4.219 (4)	P—Pb2^lxxv	4.080 (10)
Pb1—Pb2^x	4.219 (4)	P—Pb2^lxxvi	4.220 (6)
Pb1—Pb2^xi	4.219 (4)	P—Pb2^lxxvii	4.356 (10)
Pb1—Pb2^xii	4.011 (2)	P—Pb2^lxxviii	4.220 (6)
Pb1—Pb2^xiii	3.863 (8)	P—Pb2^lxxix	4.356 (10)
Pb1—Pb2^xiv	4.154 (9)	P—Pb2^lxxx	4.080 (10)
Pb1—Pb2^xv	4.154 (9)	P—Pb2^lxxxi	4.356 (10)
Pb1—Pb2^xvi	4.011 (2)	P—Pb2^lxxxii	4.080 (10)
Pb1—Pb2^xvii	3.863 (8)	P—Pb2^lxxxiii	4.220 (6)
Pb1—Pb2^xviii	3.863 (8)	P—P^lxxxiv	3.862 (15)
Pb1—Pb2^xix	4.154 (9)	P—P^li	4.232 (10)
Pb1—Pb2^xx	4.011 (2)	P—P^lii	4.232 (10)
Pb1—Pb2^xxi	3.863 (8)	P—P^liii	4.232 (10)
Pb1—Pb2^xxii	4.011 (2)	P—O1	1.515 (10)
Pb1—Pb2^xxiii	4.154 (9)	P—O1^li	3.412 (3)
Pb1—Pb2^xxiv	4.154 (9)	P—O1^lii	3.412 (3)
Pb1—Pb2^xxv	3.863 (8)	P—O1^liii	3.412 (3)
Pb1—Pb2^xxvi	4.011 (2)	P—O2^lxxxv	4.224 (8)
Pb1—Pb2^xxvii	4.011 (2)	P—O2	1.548 (5)
Pb1—Pb2^xxviii	4.154 (9)	P—O2^lxxxvi	4.345 (9)
Pb1—Pb2^xxix	3.863 (8)	P—O2^i	1.548 (5)
Pb1—Pb2^xxx	4.154 (9)	P—O2^lxxxvii	4.345 (9)
Pb1—Pb2^xxxi	3.863 (8)	P—O2^lxxxviii	4.224 (8)
Pb1—Pb2^xxxii	4.011 (2)	P—O2^lxxxix	4.345 (9)
Pb1—Pb2^xxxiii	3.863 (8)	P—O2^xc	4.224 (8)
Pb1—Pb2^xxxiv	4.011 (2)	P—O2^ii	1.548 (5)
Pb1—Pb2^xxxv	4.154 (9)	P—O2^xci	4.224 (8)
Pb1—Pb2^xxxvi	4.011 (2)	P—O2^xcii	4.345 (9)
Pb1—Pb2^xxxvii	4.154 (9)	P—O2^iii	1.548 (5)
Pb1—Pb2^xxxviii	3.863 (8)	P—O2^xciii	4.345 (9)
Pb1—Pb2^xxxix	4.154 (9)	P—O2^iv	1.548 (5)
Pb1—Pb2^xl	4.011 (2)	P—O2^xciv	4.224 (8)
Pb1—Pb2^xli	3.863 (8)	P—O2^v	1.548 (5)
Pb1—Pb2^xlii	4.011 (2)	P—O2^xcv	4.224 (8)
Pb1—Pb2^xliii	3.863 (8)	P—O2^xcvi	4.345 (9)
Pb1—Pb2^xliv	4.154 (9)	P—O2^lxxxiv	3.660 (8)
Pb1—Pb2^xlv	3.863 (8)	P—O2^xcvii	3.660 (8)
Pb1—Pb2^xlvi	4.154 (9)	P—O2^xcviii	3.660 (8)
Pb1—Pb2^xlvii	4.011 (2)	P—O2^xcix	3.660 (8)
Pb1—P^xii	3.452 (3)	P—O2^100	3.660 (8)
Pb1—P^xiii	3.452 (3)	P—O2^101	3.660 (8)
Pb1—P^xiv	3.452 (3)	P—O2^li	4.369 (11)
Pb1—P^xxx	3.452 (3)	P—O2^liii	4.250 (10)
Pb1—P^xxxi	3.452 (3)	P—O2^liv	4.250 (10)
Pb1—P^xxxii	3.452 (3)	P—O2^lv	4.369 (11)
Pb1—O1^xii	3.1512 (2)	P—O2^lvii	4.250 (10)
Pb1—O1^xiii	3.1512 (2)	P—O2^lviii	4.369 (11)
Pb1—O1^xiv	3.1512 (2)	P—O2^lix	4.369 (11)
Pb1—O1^xxx	3.1512 (2)	P—O2^lx	4.250 (10)
Pb1—O1^xxxi	3.1512 (2)	P—O2^lxi	4.250 (10)
Pb1—O1^xxxii	3.1512 (2)	P—O2^lxii	4.369 (11)
Pb1—O2^xii	4.453 (8)	P—O2^lxiii	4.369 (11)
Pb1—O2^xiii	2.560 (4)	P—O2^lxiv	4.250 (10)
Pb1—O2^xvi	4.453 (8)	O1—Pb1^xlviii	3.1512 (2)
Pb1—O2^xvii	2.560 (4)	O1—Pb1^xlix	3.1512 (2)
Pb1—O2^xviii	2.560 (4)	O1—Pb1^l	3.1512 (2)
Pb1—O2^xx	4.453 (8)	O1—Pb2	2.382 (7)
Pb1—O2^xxi	2.560 (4)	O1—Pb2^i	2.382 (7)
Pb1—O2^xxii	4.453 (8)	O1—Pb2^ii	2.382 (7)
Pb1—O2^xxv	2.560 (4)	O1—Pb2^iii	2.382 (7)
Pb1—O2^xxvi	4.453 (8)	O1—Pb2^iv	2.382 (7)
Pb1—O2^xxvii	4.453 (8)	O1—Pb2^v	2.382 (7)
Pb1—O2^xxix	2.560 (4)	O1—Pb2^li	4.075 (4)
Pb1—O2^xxxi	2.560 (4)	O1—Pb2^lii	4.215 (10)
Pb1—O2^xxxii	4.453 (8)	O1—Pb2^liii	3.929 (9)
Pb1—O2^xxxiii	2.560 (4)	O1—Pb2^liv	3.929 (9)
Pb1—O2^xxxiv	4.453 (8)	O1—Pb2^lv	4.075 (4)
Pb1—O2^xxxvi	4.453 (8)	O1—Pb2^lvi	4.215 (10)
Pb1—O2^xxxviii	2.560 (4)	O1—Pb2^lxvi	4.215 (10)
Pb1—O2^xl	4.453 (8)	O1—Pb2^lvii	3.929 (9)
Pb1—O2^xli	2.560 (4)	O1—Pb2^lviii	4.075 (4)
Pb1—O2^xlii	4.453 (8)	O1—Pb2^lxvii	4.215 (10)
Pb1—O2^xliii	2.560 (4)	O1—Pb2^lix	4.075 (4)
Pb1—O2^xlv	2.560 (4)	O1—Pb2^lx	3.929 (9)
Pb1—O2^xlvii	4.453 (8)	O1—Pb2^lxi	3.929 (9)
Pb2—Pb1	4.219 (4)	O1—Pb2^lxviii	4.215 (10)
Pb2—Pb1^xlviii	4.154 (9)	O1—Pb2^lxii	4.075 (4)
Pb2—Pb1^xlix	3.863 (8)	O1—Pb2^lxiii	4.075 (4)
Pb2—Pb1^l	4.011 (2)	O1—Pb2^lxiv	3.929 (9)
Pb2—Pb2^i	0.37 (2)	O1—Pb2^lxv	4.215 (10)
Pb2—Pb2^ii	0.37 (2)	O1—P	1.515 (10)
Pb2—Pb2^iii	0.214 (12)	O1—P^li	3.412 (3)
Pb2—Pb2^iv	0.214 (12)	O1—P^lii	3.412 (3)
Pb2—Pb2^v	0.43 (2)	O1—P^liii	3.412 (3)
Pb2—Pb2^xxx	3.93 (2)	O1—O1^li	3.1561 (7)
Pb2—Pb2^xxxi	3.286 (17)	O1—O1^lii	3.1561 (7)
Pb2—Pb2^xxxii	3.623 (5)	O1—O1^liii	3.1561 (7)
Pb2—Pb2^xxxiii	3.604 (4)	O1—O2	2.496 (6)
Pb2—Pb2^xxxiv	3.439 (9)	O1—O2^i	2.496 (6)
Pb2—Pb2^xxxv	3.762 (10)	O1—O2^ii	2.496 (6)
Pb2—Pb2^xxxvi	3.762 (10)	O1—O2^iii	2.496 (6)
Pb2—Pb2^xxxvii	3.604 (4)	O1—O2^iv	2.496 (6)
Pb2—Pb2^xxxviii	3.439 (9)	O1—O2^v	2.496 (6)
Pb2—Pb2^xxxix	3.93 (2)	O1—O2^li	3.359 (11)
Pb2—Pb2^xl	3.452 (8)	O1—O2^liii	3.202 (11)
Pb2—Pb2^xli	3.452 (8)	O1—O2^liv	3.202 (11)
Pb2—Pb2^xlii	3.774 (12)	O1—O2^lv	3.359 (11)
Pb2—Pb2^xliii	3.279 (18)	O1—O2^lvii	3.202 (11)
Pb2—Pb2^xliv	3.774 (12)	O1—O2^lviii	3.359 (11)
Pb2—Pb2^xlv	3.598 (4)	O1—O2^lix	3.359 (11)
Pb2—Pb2^xlvi	3.598 (4)	O1—O2^lx	3.202 (11)
Pb2—Pb2^xlvii	3.598 (4)	O1—O2^lxi	3.202 (11)
Pb2—P	3.894 (9)	O1—O2^lxii	3.359 (11)
Pb2—P^xii	4.220 (6)	O1—O2^lxiii	3.359 (11)
Pb2—P^xiii	4.356 (10)	O1—O2^lxiv	3.202 (11)
Pb2—P^xiv	4.080 (10)	O2—Pb1^xlix	2.560 (4)
Pb2—P^li	3.330 (2)	O2—Pb1^l	4.453 (8)
Pb2—P^lii	3.501 (10)	O2—Pb2^li	2.982 (14)
Pb2—P^liii	3.151 (11)	O2—Pb2^liii	2.587 (13)
Pb2—O1	2.382 (7)	O2—Pb2^liv	2.669 (17)
Pb2—O1^li	4.075 (4)	O2—Pb2^lvi	2.902 (17)
Pb2—O1^lii	4.215 (10)	O2—Pb2^lxvi	2.996 (14)
Pb2—O1^liii	3.929 (9)	O2—Pb2^lvii	4.464 (10)
Pb2—O2^xiii	2.962 (7)	O2—Pb2^lviii	2.604 (13)
Pb2—O2^xvii	2.743 (8)	O2—Pb2^lxvii	3.088 (17)
Pb2—O2^xviii	2.865 (5)	O2—Pb2^lx	2.485 (17)
Pb2—O2^xxi	2.851 (4)	O2—Pb2^lxi	2.772 (14)
Pb2—O2^xxv	2.969 (7)	O2—Pb2^lxii	2.796 (14)
Pb2—O2^xxvi	4.446 (12)	O2—Pb2^lxiii	2.788 (13)
Pb2—O2^xxix	2.750 (8)	O2—Pb2^lxiv	4.459 (10)
Pb2—O2^li	2.982 (14)	O2—Pb2^lxv	2.811 (14)
Pb2—O2^liii	2.587 (13)	O2—Pb2^xlix	2.962 (7)
Pb2—O2^liv	2.604 (13)	O2—Pb2^lxx	2.865 (5)
Pb2—O2^lv	2.996 (14)	O2—Pb2^lxxiii	2.743 (8)
Pb2—O2^lvi	4.464 (10)	O2—Pb2^lxxvi	2.851 (4)
Pb2—O2^lvii	2.902 (17)	O2—Pb2^lxxix	2.969 (7)
Pb2—O2^lviii	2.669 (17)	O2—Pb2^lxxx	4.446 (12)
Pb2—O2^lix	3.088 (17)	O2—Pb2^lxxxii	2.750 (8)
Pb2—O2^lx	2.485 (17)	O2—P^102	4.345 (9)
Pb2—O2^lxi	2.796 (14)	O2—P	1.548 (5)
Pb2—O2^lxii	2.772 (14)	O2—P^103	4.224 (8)
Pb2—O2^lxiii	2.788 (13)	O2—P^lxxxiv	3.660 (8)
Pb2—O2^lxiv	2.811 (14)	O2—P^li	4.369 (11)
Pb2—O2^lxv	4.459 (10)	O2—P^liii	4.250 (10)
P—Pb1^xlviii	3.452 (3)	O2—O1	2.496 (6)
P—Pb1^xlix	3.452 (3)	O2—O1^li	3.359 (11)
P—Pb1^l	3.452 (3)	O2—O1^liii	3.202 (11)
P—Pb2	3.894 (9)	O2—O2^i	2.534 (7)
P—Pb2^i	3.894 (9)	O2—O2^lxxxvii	2.931 (7)
P—Pb2^ii	3.894 (9)	O2—O2^xc	2.931 (7)
P—Pb2^iii	3.894 (9)	O2—O2^ii	2.534 (7)
P—Pb2^iv	3.894 (9)	O2—O2^xcii	3.021 (15)
P—Pb2^v	3.894 (9)	O2—O2^iii	2.434 (15)
P—Pb2^li	3.330 (2)	O2—O2^iv	0.19 (3)
P—Pb2^lii	3.501 (10)	O2—O2^v	2.623 (14)
P—Pb2^liii	3.151 (11)	O2—O2^xcv	2.832 (14)
P—Pb2^liv	3.151 (11)	O2—O2^104	4.458 (18)
P—Pb2^lv	3.330 (2)	O2—O2^lxxxiv	4.083 (8)
P—Pb2^lvi	3.501 (10)	O2—O2^105	4.220 (15)
P—Pb2^lxvi	3.501 (10)	O2—O2^xcvii	3.201 (6)
P—Pb2^lvii	3.151 (11)	O2—O2^xcviii	3.201 (6)
P—Pb2^lviii	3.330 (2)	O2—O2^xcix	3.278 (13)
P—Pb2^lxvii	3.501 (10)	O2—O2^106	4.336 (6)
P—Pb2^lix	3.330 (2)	O2—O2^100	4.079 (7)
P—Pb2^lx	3.151 (11)	O2—O2^107	4.336 (6)
P—Pb2^lxi	3.151 (11)	O2—O2^101	3.129 (10)
P—Pb2^lxviii	3.501 (10)	O2—O2^liv	4.197 (6)
P—Pb2^lxii	3.330 (2)	O2—O2^lviii	4.197 (6)
P—Pb2^lxiii	3.330 (2)	O2—O2^lx	4.133 (10)
P—Pb2^lxiv	3.151 (11)	O2—O2^lxiii	4.265 (11)
P—Pb2^lxv	3.501 (10)
Pb2^i—Pb2—Pb2^ii	60.0	O2—P—O2^i	109.8 (3)
Pb2^i—Pb2—Pb2^iii	90.0	O2—P—O2^ii	109.8 (3)
Pb2^i—Pb2—Pb2^iv	30.0000 (7)	O2—P—O2^iii	103.6 (8)
Pb2^i—Pb2—Pb2^v	30.0000 (1)	O2—P—O2^iv	7.0 (9)
Pb2^ii—Pb2—Pb2^iii	30.0000 (7)	O2—P—O2^v	115.8 (9)
Pb2^ii—Pb2—Pb2^iv	90.0	O2^i—P—O2^ii	109.8 (3)
Pb2^ii—Pb2—Pb2^v	30.0000 (1)	O2^i—P—O2^iii	115.8 (9)
Pb2^iii—Pb2—Pb2^iv	120.0000 (3)	O2^i—P—O2^iv	103.6 (8)
Pb2^iii—Pb2—Pb2^v	60.0	O2^i—P—O2^v	7.0 (9)
Pb2^iv—Pb2—Pb2^v	60.0	O2^ii—P—O2^iii	7.0 (9)
O1—P—O2	109.1 (3)	O2^ii—P—O2^iv	115.8 (9)
O1—P—O2^i	109.1 (3)	O2^ii—P—O2^v	103.6 (8)
O1—P—O2^ii	109.1 (3)	O2^iii—P—O2^iv	109.8 (3)
O1—P—O2^iii	109.1 (3)	O2^iii—P—O2^v	109.8 (3)
O1—P—O2^iv	109.1 (3)	O2^iv—P—O2^v	109.8 (3)
O1—P—O2^v	109.1 (3)	P—O2—O2^iv	86.5 (5)

Symmetry codes: (i) −y, x−y, z; (ii) y−x, −x, z; (iii) y−x, y, z; (iv) −y, −x, z; (v) x, x−y, z; (vi) −x, −y, −z; (vii) y, y−x, −z; (viii) x−y, x, −z; (ix) x−y, −y, −z; (x) y, x, −z; (xi) −x, y−x, −z; (xii) x−2/3, y−1/3, z−1/3; (xiii) x+1/3, y−1/3, z−1/3; (xiv) x+1/3, y+2/3, z−1/3; (xv) −y−2/3, x−y−1/3, z−1/3; (xvi) −y+1/3, x−y−1/3, z−1/3; (xvii) −y+1/3, x−y+2/3, z−1/3; (xviii) y−x−2/3, −x−1/3, z−1/3; (xix) y−x+1/3, −x−1/3, z−1/3; (xx) y−x+1/3, −x+2/3, z−1/3; (xxi) y−x−2/3, y−1/3, z−1/3; (xxii) y−x+1/3, y−1/3, z−1/3; (xxiii) y−x+1/3, y+2/3, z−1/3; (xxiv) −y−2/3, −x−1/3, z−1/3; (xxv) −y+1/3, −x−1/3, z−1/3; (xxvi) −y+1/3, −x+2/3, z−1/3; (xxvii) x−2/3, x−y−1/3, z−1/3; (xxviii) x+1/3, x−y−1/3, z−1/3; (xxix) x+1/3, x−y+2/3, z−1/3; (xxx) −x−2/3, −y−1/3, −z+2/3; (xxxi) −x−2/3, −y+2/3, −z+2/3; (xxxii) −x+1/3, −y+2/3, −z+2/3; (xxxiii) y−2/3, y−x−1/3, −z+2/3; (xxxiv) y−2/3, y−x+2/3, −z+2/3; (xxxv) y+1/3, y−x+2/3, −z+2/3; (xxxvi) x−y−2/3, x−1/3, −z+2/3; (xxxvii) x−y−2/3, x+2/3, −z+2/3; (xxxviii) x−y+1/3, x+2/3, −z+2/3; (xxxix) x−y−2/3, −y−1/3, −z+2/3; (xl) x−y−2/3, −y+2/3, −z+2/3; (xli) x−y+1/3, −y+2/3, −z+2/3; (xlii) y−2/3, x−1/3, −z+2/3; (xliii) y−2/3, x+2/3, −z+2/3; (xliv) y+1/3, x+2/3, −z+2/3; (xlv) −x−2/3, y−x−1/3, −z+2/3; (xlvi) −x−2/3, y−x+2/3, −z+2/3; (xlvii) −x+1/3, y−x+2/3, −z+2/3; (xlviii) x−1/3, y−2/3, z+1/3; (xlix) x−1/3, y+1/3, z+1/3; (l) x+2/3, y+1/3, z+1/3; (li) −x−1/3, −y−2/3, −z+1/3; (lii) −x+2/3, −y−2/3, −z+1/3; (liii) −x+2/3, −y+1/3, −z+1/3; (liv) y−1/3, y−x−2/3, −z+1/3; (lv) y+2/3, y−x−2/3, −z+1/3; (lvi) y+2/3, y−x+1/3, −z+1/3; (lvii) x−y+2/3, x−2/3, −z+1/3; (lviii) x−y+2/3, x+1/3, −z+1/3; (lix) x−y+2/3, −y−2/3, −z+1/3; (lx) x−y+2/3, −y+1/3, −z+1/3; (lxi) y−1/3, x−2/3, −z+1/3; (lxii) y+2/3, x+1/3, −z+1/3; (lxiii) −x−1/3, y−x−2/3, −z+1/3; (lxiv) −x+2/3, y−x−2/3, −z+1/3; (lxv) −x+2/3, y−x+1/3, −z+1/3; (lxvi) x−y−1/3, x−2/3, −z+1/3; (lxvii) x−y−1/3, −y−2/3, −z+1/3; (lxviii) y+2/3, x−2/3, −z+1/3; (lxix) −y−1/3, x−y−2/3, z+1/3; (lxx) −y−1/3, x−y+1/3, z+1/3; (lxxi) −y+2/3, x−y+1/3, z+1/3; (lxxii) y−x−1/3, −x−2/3, z+1/3; (lxxiii) y−x−1/3, −x+1/3, z+1/3; (lxxiv) y−x+2/3, −x+1/3, z+1/3; (lxxv) y−x−1/3, y−2/3, z+1/3; (lxxvi) y−x−1/3, y+1/3, z+1/3; (lxxvii) y−x+2/3, y+1/3, z+1/3; (lxxviii) −y−1/3, −x−2/3, z+1/3; (lxxix) −y−1/3, −x+1/3, z+1/3; (lxxx) −y+2/3, −x+1/3, z+1/3; (lxxxi) x−1/3, x−y−2/3, z+1/3; (lxxxii) x−1/3, x−y+1/3, z+1/3; (lxxxiii) x+2/3, x−y+1/3, z+1/3; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) −y, x−y+1, z; (lxxxviii) −y+1, x−y+1, z; (lxxxix) y−x−1, −x−1, z; (xc) y−x−1, −x, z; (xci) y−x−1, y−1, z; (xcii) y−x−1, y, z; (xciii) −y, −x−1, z; (xciv) −y+1, −x, z; (xcv) x, x−y+1, z; (xcvi) x+1, x−y+1, z; (xcvii) y, y−x, −z+1; (xcviii) x−y, x, −z+1; (xcix) x−y, −y, −z+1; (100) y, x, −z+1; (101) −x, y−x, −z+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x−1, −y, −z+1; (105) −x, −y+1, −z+1; (106) y−1, x, −z+1; (107) y, x+1, −z+1.

(S3P3X0_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8993 (6) Å	T = 298 K
c = 2.8314 (10) Å	Particle morphology: Pressure cell anvil material
V = 20.61 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.880 < d < 2.995 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.042	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 71.4 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.80 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 96.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 118.2 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.034	36 parameters
Rexp = 0.025	0 restraints
R(F^2) = 0.18318	(Δ/σ)max < 0.001
χ^2 = 1.823	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.90809 2: -0.452429 3: 0.711020 4: -0.122874 5: 0.229419 6: -0.131639 7: 0.144616 8: -0.108729 9: 0.102496 10: -7.406590E-0211: 3.979930E-0212: -1.408490E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.84934 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.219 (4)	P—Pb2	4.080 (10)
Pb1—Pb2^i	4.219 (4)	P—Pb2	4.356 (10)
Pb1—Pb2^ii	4.219 (4)	P—Pb2	4.220 (6)
Pb1—Pb2^iii	4.219 (4)	P—Pb2	4.356 (10)
Pb1—Pb2^iv	4.219 (4)	P—Pb2	4.220 (6)
Pb1—Pb2^v	4.219 (4)	P—Pb2	4.080 (10)
Pb1—Pb2	4.219 (4)	P—Pb2	4.220 (6)
Pb1—Pb2	4.219 (4)	P—Pb2	4.080 (10)
Pb1—Pb2	4.219 (4)	P—Pb2	4.356 (10)
Pb1—Pb2	4.219 (4)	P—Pb2	4.080 (10)
Pb1—Pb2	4.219 (4)	P—Pb2	4.220 (6)
Pb1—Pb2	4.219 (4)	P—Pb2	4.356 (10)
Pb1—Pb2	4.011 (2)	P—Pb2	4.220 (6)
Pb1—Pb2	3.863 (8)	P—Pb2	4.356 (10)
Pb1—Pb2	4.154 (9)	P—Pb2	4.080 (10)
Pb1—Pb2	4.154 (9)	P—Pb2	4.356 (10)
Pb1—Pb2	4.011 (2)	P—Pb2	4.080 (10)
Pb1—Pb2	3.863 (8)	P—Pb2	4.220 (6)
Pb1—Pb2	3.863 (8)	P—P	3.862 (15)
Pb1—Pb2	4.154 (9)	P—P	4.232 (10)
Pb1—Pb2	4.011 (2)	P—P	4.232 (10)
Pb1—Pb2	3.863 (8)	P—P	4.232 (10)
Pb1—Pb2	4.011 (2)	P—O1	1.515 (10)
Pb1—Pb2	4.154 (9)	P—O1	3.412 (3)
Pb1—Pb2	4.154 (9)	P—O1	3.412 (3)
Pb1—Pb2	3.863 (8)	P—O1	3.412 (3)
Pb1—Pb2	4.011 (2)	P—O2^vi	4.224 (8)
Pb1—Pb2	4.011 (2)	P—O2	1.548 (5)
Pb1—Pb2	4.154 (9)	P—O2^vii	4.345 (9)
Pb1—Pb2	3.863 (8)	P—O2^i	1.548 (5)
Pb1—Pb2	4.154 (9)	P—O2^viii	4.345 (9)
Pb1—Pb2	3.863 (8)	P—O2^ix	4.224 (8)
Pb1—Pb2	4.011 (2)	P—O2^x	4.345 (9)
Pb1—Pb2	3.863 (8)	P—O2^xi	4.224 (8)
Pb1—Pb2	4.011 (2)	P—O2^ii	1.548 (5)
Pb1—Pb2	4.154 (9)	P—O2^xii	4.224 (8)
Pb1—Pb2	4.011 (2)	P—O2^xiii	4.345 (9)
Pb1—Pb2	4.154 (9)	P—O2^iii	1.548 (5)
Pb1—Pb2	3.863 (8)	P—O2^xiv	4.345 (9)
Pb1—Pb2	4.154 (9)	P—O2^iv	1.548 (5)
Pb1—Pb2	4.011 (2)	P—O2^xv	4.224 (8)
Pb1—Pb2	3.863 (8)	P—O2^v	1.548 (5)
Pb1—Pb2	4.011 (2)	P—O2^xvi	4.224 (8)
Pb1—Pb2	3.863 (8)	P—O2^xvii	4.345 (9)
Pb1—Pb2	4.154 (9)	P—O2	3.660 (8)
Pb1—Pb2	3.863 (8)	P—O2	3.660 (8)
Pb1—Pb2	4.154 (9)	P—O2	3.660 (8)
Pb1—Pb2	4.011 (2)	P—O2	3.660 (8)
Pb1—P	3.452 (3)	P—O2	3.660 (8)
Pb1—P	3.452 (3)	P—O2	3.660 (8)
Pb1—P	3.452 (3)	P—O2	4.369 (11)
Pb1—P	3.452 (3)	P—O2	4.250 (10)
Pb1—P	3.452 (3)	P—O2	4.250 (10)
Pb1—P	3.452 (3)	P—O2	4.369 (11)
Pb1—O1	3.1512 (2)	P—O2	4.250 (10)
Pb1—O1	3.1512 (2)	P—O2	4.369 (11)
Pb1—O1	3.1512 (2)	P—O2	4.369 (11)
Pb1—O1	3.1512 (2)	P—O2	4.250 (10)
Pb1—O1	3.1512 (2)	P—O2	4.250 (10)
Pb1—O1	3.1512 (2)	P—O2	4.369 (11)
Pb1—O2	4.453 (8)	P—O2	4.369 (11)
Pb1—O2	2.560 (4)	P—O2	4.250 (10)
Pb1—O2	4.453 (8)	O1—Pb1	3.1512 (2)
Pb1—O2	2.560 (4)	O1—Pb1	3.1512 (2)
Pb1—O2	2.560 (4)	O1—Pb1	3.1512 (2)
Pb1—O2	4.453 (8)	O1—Pb2	2.382 (7)
Pb1—O2	2.560 (4)	O1—Pb2^i	2.382 (7)
Pb1—O2	4.453 (8)	O1—Pb2^ii	2.382 (7)
Pb1—O2	2.560 (4)	O1—Pb2^iii	2.382 (7)
Pb1—O2	4.453 (8)	O1—Pb2^iv	2.382 (7)
Pb1—O2	4.453 (8)	O1—Pb2^v	2.382 (7)
Pb1—O2	2.560 (4)	O1—Pb2	4.075 (4)
Pb1—O2	2.560 (4)	O1—Pb2	4.215 (10)
Pb1—O2	4.453 (8)	O1—Pb2	3.929 (9)
Pb1—O2	2.560 (4)	O1—Pb2	3.929 (9)
Pb1—O2	4.453 (8)	O1—Pb2	4.075 (4)
Pb1—O2	4.453 (8)	O1—Pb2	4.215 (10)
Pb1—O2	2.560 (4)	O1—Pb2	4.215 (10)
Pb1—O2	4.453 (8)	O1—Pb2	3.929 (9)
Pb1—O2	2.560 (4)	O1—Pb2	4.075 (4)
Pb1—O2	4.453 (8)	O1—Pb2	4.215 (10)
Pb1—O2	2.560 (4)	O1—Pb2	4.075 (4)
Pb1—O2	2.560 (4)	O1—Pb2	3.929 (9)
Pb1—O2	4.453 (8)	O1—Pb2	3.929 (9)
Pb2—Pb1	4.219 (4)	O1—Pb2	4.215 (10)
Pb2—Pb1	4.154 (9)	O1—Pb2	4.075 (4)
Pb2—Pb1	3.863 (8)	O1—Pb2	4.075 (4)
Pb2—Pb1	4.011 (2)	O1—Pb2	3.929 (9)
Pb2—Pb2^i	0.37 (2)	O1—Pb2	4.215 (10)
Pb2—Pb2^ii	0.37 (2)	O1—P	1.515 (10)
Pb2—Pb2^iii	0.214 (12)	O1—P	3.412 (3)
Pb2—Pb2^iv	0.214 (12)	O1—P	3.412 (3)
Pb2—Pb2^v	0.43 (2)	O1—P	3.412 (3)
Pb2—Pb2	3.93 (2)	O1—O1	3.1561 (7)
Pb2—Pb2	3.286 (17)	O1—O1	3.1561 (7)
Pb2—Pb2	3.623 (5)	O1—O1	3.1561 (7)
Pb2—Pb2	3.604 (4)	O1—O2	2.496 (6)
Pb2—Pb2	3.439 (9)	O1—O2^i	2.496 (6)
Pb2—Pb2	3.762 (10)	O1—O2^ii	2.496 (6)
Pb2—Pb2	3.762 (10)	O1—O2^iii	2.496 (6)
Pb2—Pb2	3.604 (4)	O1—O2^iv	2.496 (6)
Pb2—Pb2	3.439 (9)	O1—O2^v	2.496 (6)
Pb2—Pb2	3.93 (2)	O1—O2	3.359 (11)
Pb2—Pb2	3.452 (8)	O1—O2	3.202 (11)
Pb2—Pb2	3.452 (8)	O1—O2	3.202 (11)
Pb2—Pb2	3.774 (12)	O1—O2	3.359 (11)
Pb2—Pb2	3.279 (18)	O1—O2	3.202 (11)
Pb2—Pb2	3.774 (12)	O1—O2	3.359 (11)
Pb2—Pb2	3.598 (4)	O1—O2	3.359 (11)
Pb2—Pb2	3.598 (4)	O1—O2	3.202 (11)
Pb2—Pb2	3.598 (4)	O1—O2	3.202 (11)
Pb2—P	3.894 (9)	O1—O2	3.359 (11)
Pb2—P	4.220 (6)	O1—O2	3.359 (11)
Pb2—P	4.356 (10)	O1—O2	3.202 (11)
Pb2—P	4.080 (10)	O2—Pb1	2.560 (4)
Pb2—P	3.330 (2)	O2—Pb1	4.453 (8)
Pb2—P	3.501 (10)	O2—Pb2	2.982 (14)
Pb2—P	3.151 (11)	O2—Pb2	2.587 (13)
Pb2—O1	2.382 (7)	O2—Pb2	2.669 (17)
Pb2—O1	4.075 (4)	O2—Pb2	2.902 (17)
Pb2—O1	4.215 (10)	O2—Pb2	2.996 (14)
Pb2—O1	3.929 (9)	O2—Pb2	4.464 (10)
Pb2—O2	2.962 (7)	O2—Pb2	2.604 (13)
Pb2—O2	2.743 (8)	O2—Pb2	3.088 (17)
Pb2—O2	2.865 (5)	O2—Pb2	2.485 (17)
Pb2—O2	2.851 (4)	O2—Pb2	2.772 (14)
Pb2—O2	2.969 (7)	O2—Pb2	2.796 (14)
Pb2—O2	4.446 (12)	O2—Pb2	2.788 (13)
Pb2—O2	2.750 (8)	O2—Pb2	4.459 (10)
Pb2—O2	2.982 (14)	O2—Pb2	2.811 (14)
Pb2—O2	2.587 (13)	O2—Pb2	2.962 (7)
Pb2—O2	2.604 (13)	O2—Pb2	2.865 (5)
Pb2—O2	2.996 (14)	O2—Pb2	2.743 (8)
Pb2—O2	4.464 (10)	O2—Pb2	2.851 (4)
Pb2—O2	2.902 (17)	O2—Pb2	2.969 (7)
Pb2—O2	2.669 (17)	O2—Pb2	4.446 (12)
Pb2—O2	3.088 (17)	O2—Pb2	2.750 (8)
Pb2—O2	2.485 (17)	O2—P^xviii	4.345 (9)
Pb2—O2	2.796 (14)	O2—P	1.548 (5)
Pb2—O2	2.772 (14)	O2—P^xix	4.224 (8)
Pb2—O2	2.788 (13)	O2—P	3.660 (8)
Pb2—O2	2.811 (14)	O2—P	4.369 (11)
Pb2—O2	4.459 (10)	O2—P	4.250 (10)
P—Pb1	3.452 (3)	O2—O1	2.496 (6)
P—Pb1	3.452 (3)	O2—O1	3.359 (11)
P—Pb1	3.452 (3)	O2—O1	3.202 (11)
P—Pb2	3.894 (9)	O2—O2^i	2.534 (7)
P—Pb2^i	3.894 (9)	O2—O2^viii	2.931 (7)
P—Pb2^ii	3.894 (9)	O2—O2^xi	2.931 (7)
P—Pb2^iii	3.894 (9)	O2—O2^ii	2.534 (7)
P—Pb2^iv	3.894 (9)	O2—O2^xiii	3.021 (15)
P—Pb2^v	3.894 (9)	O2—O2^iii	2.434 (15)
P—Pb2	3.330 (2)	O2—O2^iv	0.19 (3)
P—Pb2	3.501 (10)	O2—O2^v	2.623 (14)
P—Pb2	3.151 (11)	O2—O2^xvi	2.832 (14)
P—Pb2	3.151 (11)	O2—O2	4.458 (18)
P—Pb2	3.330 (2)	O2—O2	4.083 (8)
P—Pb2	3.501 (10)	O2—O2	4.220 (15)
P—Pb2	3.501 (10)	O2—O2	3.201 (6)
P—Pb2	3.151 (11)	O2—O2	3.201 (6)
P—Pb2	3.330 (2)	O2—O2	3.278 (13)
P—Pb2	3.501 (10)	O2—O2	4.336 (6)
P—Pb2	3.330 (2)	O2—O2	4.079 (7)
P—Pb2	3.151 (11)	O2—O2	4.336 (6)
P—Pb2	3.151 (11)	O2—O2	3.129 (10)
P—Pb2	3.501 (10)	O2—O2	4.197 (6)
P—Pb2	3.330 (2)	O2—O2	4.197 (6)
P—Pb2	3.330 (2)	O2—O2	4.133 (10)
P—Pb2	3.151 (11)	O2—O2	4.265 (11)
P—Pb2	3.501 (10)
Pb2^i—Pb2—Pb2^ii	60.0	O2—P—O2^i	109.8 (3)
Pb2^i—Pb2—Pb2^iii	90.0	O2—P—O2^ii	109.8 (3)
Pb2^i—Pb2—Pb2^iv	30.0000 (7)	O2—P—O2^iii	103.6 (8)
Pb2^i—Pb2—Pb2^v	30.0000 (1)	O2—P—O2^iv	7.0 (9)
Pb2^ii—Pb2—Pb2^iii	30.0000 (7)	O2—P—O2^v	115.8 (9)
Pb2^ii—Pb2—Pb2^iv	90.0	O2^i—P—O2^ii	109.8 (3)
Pb2^ii—Pb2—Pb2^v	30.0000 (1)	O2^i—P—O2^iii	115.8 (9)
Pb2^iii—Pb2—Pb2^iv	120.0000 (3)	O2^i—P—O2^iv	103.6 (8)
Pb2^iii—Pb2—Pb2^v	60.0	O2^i—P—O2^v	7.0 (9)
Pb2^iv—Pb2—Pb2^v	60.0	O2^ii—P—O2^iii	7.0 (9)
O1—P—O2	109.1 (3)	O2^ii—P—O2^iv	115.8 (9)
O1—P—O2^i	109.1 (3)	O2^ii—P—O2^v	103.6 (8)
O1—P—O2^ii	109.1 (3)	O2^iii—P—O2^iv	109.8 (3)
O1—P—O2^iii	109.1 (3)	O2^iii—P—O2^v	109.8 (3)
O1—P—O2^iv	109.1 (3)	O2^iv—P—O2^v	109.8 (3)
O1—P—O2^v	109.1 (3)	P—O2—O2^iv	86.5 (5)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) x, y, −z; (iv) y−x, −x, z; (v) −y, x−y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) y−x, −x+1, −z; (ix) y−x+1, −x+1, −z; (x) −y−1, x−y−1, z; (xi) −y−1, x−y, z; (xii) x−1, y−1, −z; (xiii) x−1, y, −z; (xiv) y−x, −x−1, z; (xv) y−x+1, −x, z; (xvi) −y, x−y+1, −z; (xvii) −y+1, x−y+1, −z; (xviii) x−1, y, z; (xix) x, y+1, z.

(S3P3X0_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5382 (7) Å	Particle morphology: Component of pressure cell, not sample
V = 44.30 (3) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.880 < d < 2.995 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.042	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 71.4 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.80 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 96.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 118.2 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.034	36 parameters
Rexp = 0.025	0 restraints
R(F^2) = 0.18318	(Δ/σ)max < 0.001
χ^2 = 1.823	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.90809 2: -0.452429 3: 0.711020 4: -0.122874 5: 0.229419 6: -0.131639 7: 0.144616 8: -0.108729 9: 0.102496 10: -7.406590E-0211: 3.979930E-0212: -1.408490E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.84934 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.219 (4)	P—Pb2^xlviii	4.080 (10)
Pb1—Pb2^i	4.219 (4)	P—Pb2^xlix	4.356 (10)
Pb1—Pb2^ii	4.219 (4)	P—Pb2^l	4.220 (6)
Pb1—Pb2^iii	4.219 (4)	P—Pb2^lxix	4.356 (10)
Pb1—Pb2^iv	4.219 (4)	P—Pb2^lxx	4.220 (6)
Pb1—Pb2^v	4.219 (4)	P—Pb2^lxxi	4.080 (10)
Pb1—Pb2^vi	4.219 (4)	P—Pb2^lxxii	4.220 (6)
Pb1—Pb2^vii	4.219 (4)	P—Pb2^lxxiii	4.080 (10)
Pb1—Pb2^viii	4.219 (4)	P—Pb2^lxxiv	4.356 (10)
Pb1—Pb2^ix	4.219 (4)	P—Pb2^lxxv	4.080 (10)
Pb1—Pb2^x	4.219 (4)	P—Pb2^lxxvi	4.220 (6)
Pb1—Pb2^xi	4.219 (4)	P—Pb2^lxxvii	4.356 (10)
Pb1—Pb2^xii	4.011 (2)	P—Pb2^lxxviii	4.220 (6)
Pb1—Pb2^xiii	3.863 (8)	P—Pb2^lxxix	4.356 (10)
Pb1—Pb2^xiv	4.154 (9)	P—Pb2^lxxx	4.080 (10)
Pb1—Pb2^xv	4.154 (9)	P—Pb2^lxxxi	4.356 (10)
Pb1—Pb2^xvi	4.011 (2)	P—Pb2^lxxxii	4.080 (10)
Pb1—Pb2^xvii	3.863 (8)	P—Pb2^lxxxiii	4.220 (6)
Pb1—Pb2^xviii	3.863 (8)	P—P^lxxxiv	3.862 (15)
Pb1—Pb2^xix	4.154 (9)	P—P^li	4.232 (10)
Pb1—Pb2^xx	4.011 (2)	P—P^lii	4.232 (10)
Pb1—Pb2^xxi	3.863 (8)	P—P^liii	4.232 (10)
Pb1—Pb2^xxii	4.011 (2)	P—O1	1.515 (10)
Pb1—Pb2^xxiii	4.154 (9)	P—O1^li	3.412 (3)
Pb1—Pb2^xxiv	4.154 (9)	P—O1^lii	3.412 (3)
Pb1—Pb2^xxv	3.863 (8)	P—O1^liii	3.412 (3)
Pb1—Pb2^xxvi	4.011 (2)	P—O2^lxxxv	4.224 (8)
Pb1—Pb2^xxvii	4.011 (2)	P—O2	1.548 (5)
Pb1—Pb2^xxviii	4.154 (9)	P—O2^lxxxvi	4.345 (9)
Pb1—Pb2^xxix	3.863 (8)	P—O2^i	1.548 (5)
Pb1—Pb2^xxx	4.154 (9)	P—O2^lxxxvii	4.345 (9)
Pb1—Pb2^xxxi	3.863 (8)	P—O2^lxxxviii	4.224 (8)
Pb1—Pb2^xxxii	4.011 (2)	P—O2^lxxxix	4.345 (9)
Pb1—Pb2^xxxiii	3.863 (8)	P—O2^xc	4.224 (8)
Pb1—Pb2^xxxiv	4.011 (2)	P—O2^ii	1.548 (5)
Pb1—Pb2^xxxv	4.154 (9)	P—O2^xci	4.224 (8)
Pb1—Pb2^xxxvi	4.011 (2)	P—O2^xcii	4.345 (9)
Pb1—Pb2^xxxvii	4.154 (9)	P—O2^iii	1.548 (5)
Pb1—Pb2^xxxviii	3.863 (8)	P—O2^xciii	4.345 (9)
Pb1—Pb2^xxxix	4.154 (9)	P—O2^iv	1.548 (5)
Pb1—Pb2^xl	4.011 (2)	P—O2^xciv	4.224 (8)
Pb1—Pb2^xli	3.863 (8)	P—O2^v	1.548 (5)
Pb1—Pb2^xlii	4.011 (2)	P—O2^xcv	4.224 (8)
Pb1—Pb2^xliii	3.863 (8)	P—O2^xcvi	4.345 (9)
Pb1—Pb2^xliv	4.154 (9)	P—O2^lxxxiv	3.660 (8)
Pb1—Pb2^xlv	3.863 (8)	P—O2^xcvii	3.660 (8)
Pb1—Pb2^xlvi	4.154 (9)	P—O2^xcviii	3.660 (8)
Pb1—Pb2^xlvii	4.011 (2)	P—O2^xcix	3.660 (8)
Pb1—P^xii	3.452 (3)	P—O2^100	3.660 (8)
Pb1—P^xiii	3.452 (3)	P—O2^101	3.660 (8)
Pb1—P^xiv	3.452 (3)	P—O2^li	4.369 (11)
Pb1—P^xxx	3.452 (3)	P—O2^liii	4.250 (10)
Pb1—P^xxxi	3.452 (3)	P—O2^liv	4.250 (10)
Pb1—P^xxxii	3.452 (3)	P—O2^lv	4.369 (11)
Pb1—O1^xii	3.1512 (2)	P—O2^lvii	4.250 (10)
Pb1—O1^xiii	3.1512 (2)	P—O2^lviii	4.369 (11)
Pb1—O1^xiv	3.1512 (2)	P—O2^lix	4.369 (11)
Pb1—O1^xxx	3.1512 (2)	P—O2^lx	4.250 (10)
Pb1—O1^xxxi	3.1512 (2)	P—O2^lxi	4.250 (10)
Pb1—O1^xxxii	3.1512 (2)	P—O2^lxii	4.369 (11)
Pb1—O2^xii	4.453 (8)	P—O2^lxiii	4.369 (11)
Pb1—O2^xiii	2.560 (4)	P—O2^lxiv	4.250 (10)
Pb1—O2^xvi	4.453 (8)	O1—Pb1^xlviii	3.1512 (2)
Pb1—O2^xvii	2.560 (4)	O1—Pb1^xlix	3.1512 (2)
Pb1—O2^xviii	2.560 (4)	O1—Pb1^l	3.1512 (2)
Pb1—O2^xx	4.453 (8)	O1—Pb2	2.382 (7)
Pb1—O2^xxi	2.560 (4)	O1—Pb2^i	2.382 (7)
Pb1—O2^xxii	4.453 (8)	O1—Pb2^ii	2.382 (7)
Pb1—O2^xxv	2.560 (4)	O1—Pb2^iii	2.382 (7)
Pb1—O2^xxvi	4.453 (8)	O1—Pb2^iv	2.382 (7)
Pb1—O2^xxvii	4.453 (8)	O1—Pb2^v	2.382 (7)
Pb1—O2^xxix	2.560 (4)	O1—Pb2^li	4.075 (4)
Pb1—O2^xxxi	2.560 (4)	O1—Pb2^lii	4.215 (10)
Pb1—O2^xxxii	4.453 (8)	O1—Pb2^liii	3.929 (9)
Pb1—O2^xxxiii	2.560 (4)	O1—Pb2^liv	3.929 (9)
Pb1—O2^xxxiv	4.453 (8)	O1—Pb2^lv	4.075 (4)
Pb1—O2^xxxvi	4.453 (8)	O1—Pb2^lvi	4.215 (10)
Pb1—O2^xxxviii	2.560 (4)	O1—Pb2^lxvi	4.215 (10)
Pb1—O2^xl	4.453 (8)	O1—Pb2^lvii	3.929 (9)
Pb1—O2^xli	2.560 (4)	O1—Pb2^lviii	4.075 (4)
Pb1—O2^xlii	4.453 (8)	O1—Pb2^lxvii	4.215 (10)
Pb1—O2^xliii	2.560 (4)	O1—Pb2^lix	4.075 (4)
Pb1—O2^xlv	2.560 (4)	O1—Pb2^lx	3.929 (9)
Pb1—O2^xlvii	4.453 (8)	O1—Pb2^lxi	3.929 (9)
Pb2—Pb1	4.219 (4)	O1—Pb2^lxviii	4.215 (10)
Pb2—Pb1^xlviii	4.154 (9)	O1—Pb2^lxii	4.075 (4)
Pb2—Pb1^xlix	3.863 (8)	O1—Pb2^lxiii	4.075 (4)
Pb2—Pb1^l	4.011 (2)	O1—Pb2^lxiv	3.929 (9)
Pb2—Pb2^i	0.37 (2)	O1—Pb2^lxv	4.215 (10)
Pb2—Pb2^ii	0.37 (2)	O1—P	1.515 (10)
Pb2—Pb2^iii	0.214 (12)	O1—P^li	3.412 (3)
Pb2—Pb2^iv	0.214 (12)	O1—P^lii	3.412 (3)
Pb2—Pb2^v	0.43 (2)	O1—P^liii	3.412 (3)
Pb2—Pb2^xxx	3.93 (2)	O1—O1^li	3.1561 (7)
Pb2—Pb2^xxxi	3.286 (17)	O1—O1^lii	3.1561 (7)
Pb2—Pb2^xxxii	3.623 (5)	O1—O1^liii	3.1561 (7)
Pb2—Pb2^xxxiii	3.604 (4)	O1—O2	2.496 (6)
Pb2—Pb2^xxxiv	3.439 (9)	O1—O2^i	2.496 (6)
Pb2—Pb2^xxxv	3.762 (10)	O1—O2^ii	2.496 (6)
Pb2—Pb2^xxxvi	3.762 (10)	O1—O2^iii	2.496 (6)
Pb2—Pb2^xxxvii	3.604 (4)	O1—O2^iv	2.496 (6)
Pb2—Pb2^xxxviii	3.439 (9)	O1—O2^v	2.496 (6)
Pb2—Pb2^xxxix	3.93 (2)	O1—O2^li	3.359 (11)
Pb2—Pb2^xl	3.452 (8)	O1—O2^liii	3.202 (11)
Pb2—Pb2^xli	3.452 (8)	O1—O2^liv	3.202 (11)
Pb2—Pb2^xlii	3.774 (12)	O1—O2^lv	3.359 (11)
Pb2—Pb2^xliii	3.279 (18)	O1—O2^lvii	3.202 (11)
Pb2—Pb2^xliv	3.774 (12)	O1—O2^lviii	3.359 (11)
Pb2—Pb2^xlv	3.598 (4)	O1—O2^lix	3.359 (11)
Pb2—Pb2^xlvi	3.598 (4)	O1—O2^lx	3.202 (11)
Pb2—Pb2^xlvii	3.598 (4)	O1—O2^lxi	3.202 (11)
Pb2—P	3.894 (9)	O1—O2^lxii	3.359 (11)
Pb2—P^xii	4.220 (6)	O1—O2^lxiii	3.359 (11)
Pb2—P^xiii	4.356 (10)	O1—O2^lxiv	3.202 (11)
Pb2—P^xiv	4.080 (10)	O2—Pb1^xlix	2.560 (4)
Pb2—P^li	3.330 (2)	O2—Pb1^l	4.453 (8)
Pb2—P^lii	3.501 (10)	O2—Pb2^li	2.982 (14)
Pb2—P^liii	3.151 (11)	O2—Pb2^liii	2.587 (13)
Pb2—O1	2.382 (7)	O2—Pb2^liv	2.669 (17)
Pb2—O1^li	4.075 (4)	O2—Pb2^lvi	2.902 (17)
Pb2—O1^lii	4.215 (10)	O2—Pb2^lxvi	2.996 (14)
Pb2—O1^liii	3.929 (9)	O2—Pb2^lvii	4.464 (10)
Pb2—O2^xiii	2.962 (7)	O2—Pb2^lviii	2.604 (13)
Pb2—O2^xvii	2.743 (8)	O2—Pb2^lxvii	3.088 (17)
Pb2—O2^xviii	2.865 (5)	O2—Pb2^lx	2.485 (17)
Pb2—O2^xxi	2.851 (4)	O2—Pb2^lxi	2.772 (14)
Pb2—O2^xxv	2.969 (7)	O2—Pb2^lxii	2.796 (14)
Pb2—O2^xxvi	4.446 (12)	O2—Pb2^lxiii	2.788 (13)
Pb2—O2^xxix	2.750 (8)	O2—Pb2^lxiv	4.459 (10)
Pb2—O2^li	2.982 (14)	O2—Pb2^lxv	2.811 (14)
Pb2—O2^liii	2.587 (13)	O2—Pb2^xlix	2.962 (7)
Pb2—O2^liv	2.604 (13)	O2—Pb2^lxx	2.865 (5)
Pb2—O2^lv	2.996 (14)	O2—Pb2^lxxiii	2.743 (8)
Pb2—O2^lvi	4.464 (10)	O2—Pb2^lxxvi	2.851 (4)
Pb2—O2^lvii	2.902 (17)	O2—Pb2^lxxix	2.969 (7)
Pb2—O2^lviii	2.669 (17)	O2—Pb2^lxxx	4.446 (12)
Pb2—O2^lix	3.088 (17)	O2—Pb2^lxxxii	2.750 (8)
Pb2—O2^lx	2.485 (17)	O2—P^102	4.345 (9)
Pb2—O2^lxi	2.796 (14)	O2—P	1.548 (5)
Pb2—O2^lxii	2.772 (14)	O2—P^103	4.224 (8)
Pb2—O2^lxiii	2.788 (13)	O2—P^lxxxiv	3.660 (8)
Pb2—O2^lxiv	2.811 (14)	O2—P^li	4.369 (11)
Pb2—O2^lxv	4.459 (10)	O2—P^liii	4.250 (10)
P—Pb1^xlviii	3.452 (3)	O2—O1	2.496 (6)
P—Pb1^xlix	3.452 (3)	O2—O1^li	3.359 (11)
P—Pb1^l	3.452 (3)	O2—O1^liii	3.202 (11)
P—Pb2	3.894 (9)	O2—O2^i	2.534 (7)
P—Pb2^i	3.894 (9)	O2—O2^lxxxvii	2.931 (7)
P—Pb2^ii	3.894 (9)	O2—O2^xc	2.931 (7)
P—Pb2^iii	3.894 (9)	O2—O2^ii	2.534 (7)
P—Pb2^iv	3.894 (9)	O2—O2^xcii	3.021 (15)
P—Pb2^v	3.894 (9)	O2—O2^iii	2.434 (15)
P—Pb2^li	3.330 (2)	O2—O2^iv	0.19 (3)
P—Pb2^lii	3.501 (10)	O2—O2^v	2.623 (14)
P—Pb2^liii	3.151 (11)	O2—O2^xcv	2.832 (14)
P—Pb2^liv	3.151 (11)	O2—O2^104	4.458 (18)
P—Pb2^lv	3.330 (2)	O2—O2^lxxxiv	4.083 (8)
P—Pb2^lvi	3.501 (10)	O2—O2^105	4.220 (15)
P—Pb2^lxvi	3.501 (10)	O2—O2^xcvii	3.201 (6)
P—Pb2^lvii	3.151 (11)	O2—O2^xcviii	3.201 (6)
P—Pb2^lviii	3.330 (2)	O2—O2^xcix	3.278 (13)
P—Pb2^lxvii	3.501 (10)	O2—O2^106	4.336 (6)
P—Pb2^lix	3.330 (2)	O2—O2^100	4.079 (7)
P—Pb2^lx	3.151 (11)	O2—O2^107	4.336 (6)
P—Pb2^lxi	3.151 (11)	O2—O2^101	3.129 (10)
P—Pb2^lxviii	3.501 (10)	O2—O2^liv	4.197 (6)
P—Pb2^lxii	3.330 (2)	O2—O2^lviii	4.197 (6)
P—Pb2^lxiii	3.330 (2)	O2—O2^lx	4.133 (10)
P—Pb2^lxiv	3.151 (11)	O2—O2^lxiii	4.265 (11)
P—Pb2^lxv	3.501 (10)
Pb2^i—Pb2—Pb2^ii	60.0	O2—P—O2^i	109.8 (3)
Pb2^i—Pb2—Pb2^iii	90.0	O2—P—O2^ii	109.8 (3)
Pb2^i—Pb2—Pb2^iv	30.0000 (7)	O2—P—O2^iii	103.6 (8)
Pb2^i—Pb2—Pb2^v	30.0000 (1)	O2—P—O2^iv	7.0 (9)
Pb2^ii—Pb2—Pb2^iii	30.0000 (7)	O2—P—O2^v	115.8 (9)
Pb2^ii—Pb2—Pb2^iv	90.0	O2^i—P—O2^ii	109.8 (3)
Pb2^ii—Pb2—Pb2^v	30.0000 (1)	O2^i—P—O2^iii	115.8 (9)
Pb2^iii—Pb2—Pb2^iv	120.0000 (3)	O2^i—P—O2^iv	103.6 (8)
Pb2^iii—Pb2—Pb2^v	60.0	O2^i—P—O2^v	7.0 (9)
Pb2^iv—Pb2—Pb2^v	60.0	O2^ii—P—O2^iii	7.0 (9)
O1—P—O2	109.1 (3)	O2^ii—P—O2^iv	115.8 (9)
O1—P—O2^i	109.1 (3)	O2^ii—P—O2^v	103.6 (8)
O1—P—O2^ii	109.1 (3)	O2^iii—P—O2^iv	109.8 (3)
O1—P—O2^iii	109.1 (3)	O2^iii—P—O2^v	109.8 (3)
O1—P—O2^iv	109.1 (3)	O2^iv—P—O2^v	109.8 (3)
O1—P—O2^v	109.1 (3)	P—O2—O2^iv	86.5 (5)

Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) x, y, −z; (iv) −z, x, y; (v) y, −z, x; (vi) −x, −y, −z; (vii) −z, −x, −y; (viii) −y, −z, −x; (ix) −x, −y, z; (x) z, −x, −y; (xi) −y, z, −x; (xii) x−1, y−1/2, z−1/2; (xiii) x, y−1/2, z−1/2; (xiv) x, y+1/2, z−1/2; (xv) z−1, x−1/2, y−1/2; (xvi) z, x−1/2, y−1/2; (xvii) z, x+1/2, y−1/2; (xviii) y−1, z−1/2, x−1/2; (xix) y, z−1/2, x−1/2; (xx) y, z+1/2, x−1/2; (xxi) x−1, y−1/2, −z−1/2; (xxii) x, y−1/2, −z−1/2; (xxiii) x, y+1/2, −z−1/2; (xxiv) −z−1, x−1/2, y−1/2; (xxv) −z, x−1/2, y−1/2; (xxvi) −z, x+1/2, y−1/2; (xxvii) y−1, −z−1/2, x−1/2; (xxviii) y, −z−1/2, x−1/2; (xxix) y, −z+1/2, x−1/2; (xxx) −x−1/2, −y−1, −z+1/2; (xxxi) −x−1/2, −y, −z+1/2; (xxxii) −x+1/2, −y, −z+1/2; (xxxiii) −z−1/2, −x−1, −y+1/2; (xxxiv) −z−1/2, −x, −y+1/2; (xxxv) −z+1/2, −x, −y+1/2; (xxxvi) −y−1/2, −z−1, −x+1/2; (xxxvii) −y−1/2, −z, −x+1/2; (xxxviii) −y+1/2, −z, −x+1/2; (xxxix) −x−1/2, −y−1, z+1/2; (xl) −x−1/2, −y, z+1/2; (xli) −x+1/2, −y, z+1/2; (xlii) z−1/2, −x−1, −y+1/2; (xliii) z−1/2, −x, −y+1/2; (xliv) z+1/2, −x, −y+1/2; (xlv) −y−1/2, z−1, −x+1/2; (xlvi) −y−1/2, z, −x+1/2; (xlvii) −y+1/2, z, −x+1/2; (xlviii) x−1/2, y−1, z+1/2; (xlix) x−1/2, y, z+1/2; (l) x+1/2, y, z+1/2; (li) −x−1, −y−1/2, −z+1/2; (lii) −x, −y−1/2, −z+1/2; (liii) −x, −y+1/2, −z+1/2; (liv) −z−1, −x−1/2, −y+1/2; (lv) −z, −x−1/2, −y+1/2; (lvi) −z, −x+1/2, −y+1/2; (lvii) −y, −z−1/2, −x+1/2; (lviii) −y, −z+1/2, −x+1/2; (lix) −x, −y−1/2, z+1/2; (lx) −x, −y+1/2, z+1/2; (lxi) z−1, −x−1/2, −y+1/2; (lxii) z, −x+1/2, −y+1/2; (lxiii) −y−1, z−1/2, −x+1/2; (lxiv) −y, z−1/2, −x+1/2; (lxv) −y, z+1/2, −x+1/2; (lxvi) −y−1, −z−1/2, −x+1/2; (lxvii) −x−1, −y−1/2, z+1/2; (lxviii) z, −x−1/2, −y+1/2; (lxix) z−1/2, x−1, y+1/2; (lxx) z−1/2, x, y+1/2; (lxxi) z+1/2, x, y+1/2; (lxxii) y−1/2, z−1, x+1/2; (lxxiii) y−1/2, z, x+1/2; (lxxiv) y+1/2, z, x+1/2; (lxxv) x−1/2, y−1, −z+1/2; (lxxvi) x−1/2, y, −z+1/2; (lxxvii) x+1/2, y, −z+1/2; (lxxviii) −z−1/2, x−1, y+1/2; (lxxix) −z−1/2, x, y+1/2; (lxxx) −z+1/2, x, y+1/2; (lxxxi) y−1/2, −z−1, x+1/2; (lxxxii) y−1/2, −z, x+1/2; (lxxxiii) y+1/2, −z, x+1/2; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) z, x+1, y; (lxxxviii) z+1, x+1, y; (lxxxix) y−1, z−1, x; (xc) y−1, z, x; (xci) x−1, y−1, −z; (xcii) x−1, y, −z; (xciii) −z, x−1, y; (xciv) −z+1, x, y; (xcv) y, −z+1, x; (xcvi) y+1, −z+1, x; (xcvii) −z, −x, −y+1; (xcviii) −y, −z, −x+1; (xcix) −x, −y, z+1; (100) z, −x, −y+1; (101) −y, z, −x+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x−1, −y, −z+1; (105) −x, −y+1, −z+1; (106) z−1, −x, −y+1; (107) z, −x+1, −y+1.

(S3P4X0_phase_1)

Crystal data

O8.00P2Pb3.00	Z = 3
Mr = 811.74	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.42360 (19) Å	Particle morphology: plate
c = 19.9856 (11) Å	irregular, 6 × 6 mm
V = 509.12 (4) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.881 < d < 2.998 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.040	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 60.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.02 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 123.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 248.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.032	36 parameters
Rexp = 0.023	0 restraints
R(F^2) = 0.17019	(Δ/σ)max = 0.01
χ^2 = 1.932	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 2.23627 2: -0.566994 3: 0.896526 4: -0.182112 5: 0.350911 6: -0.196381 7: 0.201360 8: -0.135196 9: 0.125708 10: -9.856300E-0211: 5.324140E-0212: -2.400480E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.80545 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pb1	0.0	0.0	0.0	0.0250 (16)*
Pb2	0.0	0.019 (4)	0.20951 (16)	0.0250 (16)*	0.16667
P	0.0	0.0	0.4033 (3)	0.0111 (13)*
O1	0.0	0.0	0.3286 (2)	0.0177 (10)*
O2	−0.143 (3)	0.167 (3)	0.42961 (15)	0.0177 (10)*	0.5

Geometric parameters (Å, º)

Pb1—Pb2	4.188 (3)	P—Pb2^lv	3.313 (2)
Pb1—Pb2^i	4.188 (3)	P—Pb2^lxiv	3.396 (19)
Pb1—Pb2^ii	4.188 (3)	P—Pb2^lxv	3.396 (19)
Pb1—Pb2^iii	4.188 (3)	P—Pb2^lvi	3.228 (19)
Pb1—Pb2^iv	4.188 (3)	P—Pb2^lvii	3.313 (2)
Pb1—Pb2^v	4.188 (3)	P—Pb2^lxvi	3.396 (19)
Pb1—Pb2^vi	4.188 (3)	P—Pb2^lviii	3.313 (2)
Pb1—Pb2^vii	4.188 (3)	P—Pb2^lix	3.228 (19)
Pb1—Pb2^viii	4.188 (3)	P—Pb2^lx	3.228 (19)
Pb1—Pb2^ix	4.188 (3)	P—Pb2^lxvii	3.396 (19)
Pb1—Pb2^x	4.188 (3)	P—Pb2^lxi	3.313 (2)
Pb1—Pb2^xi	4.188 (3)	P—Pb2^lxii	3.313 (2)
Pb1—Pb2^xii	3.993 (2)	P—Pb2^lxiii	3.228 (19)
Pb1—Pb2^xiii	3.922 (16)	P—Pb2^lxviii	3.396 (19)
Pb1—Pb2^xiv	4.062 (16)	P—Pb2^xlviii	4.128 (16)
Pb1—Pb2^xv	4.062 (16)	P—Pb2^l	4.195 (5)
Pb1—Pb2^xvi	3.993 (2)	P—Pb2^lxix	4.195 (5)
Pb1—Pb2^xvii	3.922 (16)	P—Pb2^lxx	4.128 (16)
Pb1—Pb2^xviii	3.922 (16)	P—Pb2^lxxi	4.195 (5)
Pb1—Pb2^xix	4.062 (16)	P—Pb2^lxxii	4.128 (16)
Pb1—Pb2^xx	3.993 (2)	P—Pb2^lxxiii	4.128 (16)
Pb1—Pb2^xxi	3.922 (16)	P—Pb2^lxxiv	4.195 (5)
Pb1—Pb2^xxii	3.993 (2)	P—Pb2^lxxv	4.195 (5)
Pb1—Pb2^xxiii	4.062 (16)	P—Pb2^lxxvi	4.128 (16)
Pb1—Pb2^xxiv	4.062 (16)	P—Pb2^lxxvii	4.128 (16)
Pb1—Pb2^xxv	3.922 (16)	P—Pb2^lxxviii	4.195 (5)
Pb1—Pb2^xxvi	3.993 (2)	P—P^lxxix	3.867 (13)
Pb1—Pb2^xxvii	3.993 (2)	P—P^li	4.197 (9)
Pb1—Pb2^xxviii	4.062 (16)	P—P^lii	4.197 (9)
Pb1—Pb2^xxix	3.922 (16)	P—P^liii	4.197 (9)
Pb1—Pb2^xxx	4.062 (16)	P—O1	1.491 (9)
Pb1—Pb2^xxxi	3.922 (16)	P—O1^li	3.392 (3)
Pb1—Pb2^xxxii	3.993 (2)	P—O1^lii	3.392 (3)
Pb1—Pb2^xxxiii	3.922 (16)	P—O1^liii	3.392 (3)
Pb1—Pb2^xxxiv	3.993 (2)	P—O2	1.546 (4)
Pb1—Pb2^xxxv	4.062 (16)	P—O2^i	1.546 (4)
Pb1—Pb2^xxxvi	3.993 (2)	P—O2^ii	1.546 (4)
Pb1—Pb2^xxxvii	4.062 (16)	P—O2^iii	1.546 (4)
Pb1—Pb2^xxxviii	3.922 (16)	P—O2^iv	1.546 (4)
Pb1—Pb2^xxxix	4.062 (16)	P—O2^v	1.546 (4)
Pb1—Pb2^xl	3.993 (2)	P—O2^lxxix	3.643 (7)
Pb1—Pb2^xli	3.922 (16)	P—O2^lxxx	3.643 (7)
Pb1—Pb2^xlii	3.993 (2)	P—O2^lxxxi	3.643 (7)
Pb1—Pb2^xliii	3.922 (16)	P—O2^lxxxii	3.643 (7)
Pb1—Pb2^xliv	4.062 (16)	P—O2^lxxxiii	3.643 (7)
Pb1—Pb2^xlv	3.922 (16)	P—O2^lxxxiv	3.643 (7)
Pb1—Pb2^xlvi	4.062 (16)	O1—Pb1^xlviii	3.1327 (2)
Pb1—Pb2^xlvii	3.993 (2)	O1—Pb1^xlix	3.1327 (2)
Pb1—P^xii	3.429 (3)	O1—Pb1^l	3.1327 (2)
Pb1—P^xiii	3.429 (3)	O1—Pb2	2.383 (6)
Pb1—P^xiv	3.429 (3)	O1—Pb2^i	2.383 (6)
Pb1—P^xxx	3.429 (3)	O1—Pb2^ii	2.383 (6)
Pb1—P^xxxi	3.429 (3)	O1—Pb2^iii	2.383 (6)
Pb1—P^xxxii	3.429 (3)	O1—Pb2^iv	2.383 (6)
Pb1—O1^xii	3.1327 (2)	O1—Pb2^v	2.383 (6)
Pb1—O1^xiii	3.1327 (2)	O1—Pb2^li	4.051 (4)
Pb1—O1^xiv	3.1327 (2)	O1—Pb2^lii	4.120 (17)
Pb1—O1^xxx	3.1327 (2)	O1—Pb2^liii	3.982 (15)
Pb1—O1^xxxi	3.1327 (2)	O1—Pb2^liv	3.982 (15)
Pb1—O1^xxxii	3.1327 (2)	O1—Pb2^lv	4.051 (4)
Pb1—O2^xiii	2.555 (3)	O1—Pb2^lxiv	4.120 (17)
Pb1—O2^xvii	2.555 (3)	O1—Pb2^lxv	4.120 (17)
Pb1—O2^xviii	2.555 (3)	O1—Pb2^lvi	3.982 (15)
Pb1—O2^xxi	2.555 (3)	O1—Pb2^lvii	4.051 (4)
Pb1—O2^xxv	2.555 (3)	O1—Pb2^lxvi	4.120 (17)
Pb1—O2^xxix	2.555 (3)	O1—Pb2^lviii	4.051 (4)
Pb1—O2^xxxi	2.555 (3)	O1—Pb2^lix	3.982 (15)
Pb1—O2^xxxiii	2.555 (3)	O1—Pb2^lx	3.982 (15)
Pb1—O2^xxxviii	2.555 (3)	O1—Pb2^lxvii	4.120 (17)
Pb1—O2^xli	2.555 (3)	O1—Pb2^lxi	4.051 (4)
Pb1—O2^xliii	2.555 (3)	O1—Pb2^lxii	4.051 (4)
Pb1—O2^xlv	2.555 (3)	O1—Pb2^lxiii	3.982 (15)
Pb2—Pb1	4.188 (3)	O1—Pb2^lxviii	4.120 (17)
Pb2—Pb1^xlviii	4.062 (16)	O1—P	1.491 (9)
Pb2—Pb1^xlix	3.922 (16)	O1—P^li	3.392 (3)
Pb2—Pb1^l	3.993 (2)	O1—P^lii	3.392 (3)
Pb2—Pb2^i	0.18 (4)	O1—P^liii	3.392 (3)
Pb2—Pb2^ii	0.18 (4)	O1—O1^li	3.1369 (6)
Pb2—Pb2^iii	0.10 (2)	O1—O1^lii	3.1369 (6)
Pb2—Pb2^iv	0.10 (2)	O1—O1^liii	3.1369 (6)
Pb2—Pb2^v	0.21 (5)	O1—O2	2.487 (5)
Pb2—Pb2^xxx	3.73 (4)	O1—O2^i	2.487 (5)
Pb2—Pb2^xxxi	3.42 (3)	O1—O2^ii	2.487 (5)
Pb2—Pb2^xxxii	3.575 (4)	O1—O2^iii	2.487 (5)
Pb2—Pb2^xxxiii	3.571 (3)	O1—O2^iv	2.487 (5)
Pb2—Pb2^xxxiv	3.491 (17)	O1—O2^v	2.487 (5)
Pb2—Pb2^xxxv	3.648 (19)	O1—O2^li	3.328 (13)
Pb2—Pb2^xxxvi	3.648 (19)	O1—O2^liii	3.220 (14)
Pb2—Pb2^xxxvii	3.571 (3)	O1—O2^liv	3.220 (14)
Pb2—Pb2^xxxviii	3.491 (17)	O1—O2^lv	3.328 (13)
Pb2—Pb2^xxxix	3.73 (4)	O1—O2^lvi	3.220 (14)
Pb2—Pb2^xl	3.494 (16)	O1—O2^lvii	3.328 (13)
Pb2—Pb2^xli	3.494 (16)	O1—O2^lviii	3.328 (13)
Pb2—Pb2^xlii	3.65 (2)	O1—O2^lix	3.220 (14)
Pb2—Pb2^xliii	3.41 (4)	O1—O2^lx	3.220 (14)
Pb2—Pb2^xliv	3.65 (2)	O1—O2^lxi	3.328 (13)
Pb2—Pb2^xlv	3.569 (3)	O1—O2^lxii	3.328 (13)
Pb2—Pb2^xlvi	3.569 (3)	O1—O2^lxiii	3.220 (14)
Pb2—Pb2^xlvii	3.569 (3)	O2—Pb1^xlix	2.555 (3)
Pb2—P	3.874 (8)	O2—Pb2^li	2.882 (18)
Pb2—P^xii	4.195 (5)	O2—Pb2^liii	2.653 (19)
Pb2—P^xiv	4.128 (16)	O2—Pb2^liv	2.73 (3)
Pb2—P^li	3.313 (2)	O2—Pb2^lxiv	2.81 (3)
Pb2—P^lii	3.396 (19)	O2—Pb2^lxv	2.889 (19)
Pb2—P^liii	3.228 (19)	O2—Pb2^lvii	2.661 (18)
Pb2—O1	2.383 (6)	O2—Pb2^lxvi	2.94 (3)
Pb2—O1^li	4.051 (4)	O2—Pb2^lix	2.61 (3)
Pb2—O1^lii	4.120 (17)	O2—Pb2^lx	2.78 (2)
Pb2—O1^liii	3.982 (15)	O2—Pb2^lxi	2.75 (2)
Pb2—O2^xiii	2.872 (12)	O2—Pb2^lxii	2.788 (19)
Pb2—O2^xvii	2.766 (13)	O2—Pb2^lxviii	2.76 (2)
Pb2—O2^xviii	2.823 (4)	O2—Pb2^xlix	2.872 (12)
Pb2—O2^xxi	2.818 (4)	O2—Pb2^lxix	2.823 (4)
Pb2—O2^xxv	2.875 (12)	O2—Pb2^lxxii	2.766 (13)
Pb2—O2^xxix	2.768 (13)	O2—Pb2^lxxiv	2.818 (4)
Pb2—O2^li	2.882 (18)	O2—Pb2^lxxxv	2.875 (12)
Pb2—O2^liii	2.653 (19)	O2—Pb2^lxxvii	2.768 (13)
Pb2—O2^liv	2.661 (18)	O2—P	1.546 (4)
Pb2—O2^lv	2.889 (19)	O2—P^lxxix	3.643 (7)
Pb2—O2^lvi	2.81 (3)	O2—O1	2.487 (5)
Pb2—O2^lvii	2.73 (3)	O2—O1^li	3.328 (13)
Pb2—O2^lviii	2.94 (3)	O2—O1^liii	3.220 (14)
Pb2—O2^lix	2.61 (3)	O2—O2^i	2.517 (6)
Pb2—O2^lx	2.75 (2)	O2—O2^lxxxvi	2.911 (6)
Pb2—O2^lxi	2.78 (2)	O2—O2^lxxxvii	2.911 (6)
Pb2—O2^lxii	2.788 (19)	O2—O2^ii	2.517 (6)
Pb2—O2^lxiii	2.76 (2)	O2—O2^lxxxviii	2.974 (17)
P—Pb1^xlviii	3.429 (3)	O2—O2^iii	2.449 (17)
P—Pb1^xlix	3.429 (3)	O2—O2^iv	0.13 (3)
P—Pb1^l	3.429 (3)	O2—O2^v	2.580 (17)
P—Pb2	3.874 (8)	O2—O2^lxxxix	2.844 (17)
P—Pb2^i	3.874 (8)	O2—O2^lxxix	4.045 (7)
P—Pb2^ii	3.874 (8)	O2—O2^lxxx	3.167 (5)
P—Pb2^iii	3.874 (8)	O2—O2^lxxxi	3.167 (5)
P—Pb2^iv	3.874 (8)	O2—O2^lxxxii	3.219 (15)
P—Pb2^v	3.874 (8)	O2—O2^lxxxiii	4.043 (7)
P—Pb2^li	3.313 (2)	O2—O2^lxxxiv	3.116 (13)
P—Pb2^lii	3.396 (19)	O2—O2^liv	4.199 (6)
P—Pb2^liii	3.228 (19)	O2—O2^lvii	4.199 (6)
P—Pb2^liv	3.228 (19)	O2—O2^lix	4.155 (12)
O1—P—O2	109.9 (3)	O2^i—P—O2^ii	109.0 (3)
O1—P—O2^i	109.9 (3)	O2^i—P—O2^iii	113.1 (10)
O1—P—O2^ii	109.9 (3)	O2^i—P—O2^iv	104.8 (10)
O1—P—O2^iii	109.9 (3)	O2^i—P—O2^v	4.8 (12)
O1—P—O2^iv	109.9 (3)	O2^ii—P—O2^iii	4.8 (12)
O1—P—O2^v	109.9 (3)	O2^ii—P—O2^iv	113.1 (10)
O2—P—O2^i	109.0 (3)	O2^ii—P—O2^v	104.8 (10)
O2—P—O2^ii	109.0 (3)	O2^iii—P—O2^iv	109.0 (3)
O2—P—O2^iii	104.8 (10)	O2^iii—P—O2^v	109.0 (3)
O2—P—O2^iv	4.8 (12)	O2^iv—P—O2^v	109.0 (3)
O2—P—O2^v	113.1 (10)	P—O2—O2^iv	87.6 (6)

Symmetry codes: (i) −y, x−y, z; (ii) y−x, −x, z; (iii) y−x, y, z; (iv) −y, −x, z; (v) x, x−y, z; (vi) −x, −y, −z; (vii) y, y−x, −z; (viii) x−y, x, −z; (ix) x−y, −y, −z; (x) y, x, −z; (xi) −x, y−x, −z; (xii) x−2/3, y−1/3, z−1/3; (xiii) x+1/3, y−1/3, z−1/3; (xiv) x+1/3, y+2/3, z−1/3; (xv) −y−2/3, x−y−1/3, z−1/3; (xvi) −y+1/3, x−y−1/3, z−1/3; (xvii) −y+1/3, x−y+2/3, z−1/3; (xviii) y−x−2/3, −x−1/3, z−1/3; (xix) y−x+1/3, −x−1/3, z−1/3; (xx) y−x+1/3, −x+2/3, z−1/3; (xxi) y−x−2/3, y−1/3, z−1/3; (xxii) y−x+1/3, y−1/3, z−1/3; (xxiii) y−x+1/3, y+2/3, z−1/3; (xxiv) −y−2/3, −x−1/3, z−1/3; (xxv) −y+1/3, −x−1/3, z−1/3; (xxvi) −y+1/3, −x+2/3, z−1/3; (xxvii) x−2/3, x−y−1/3, z−1/3; (xxviii) x+1/3, x−y−1/3, z−1/3; (xxix) x+1/3, x−y+2/3, z−1/3; (xxx) −x−2/3, −y−1/3, −z+2/3; (xxxi) −x−2/3, −y+2/3, −z+2/3; (xxxii) −x+1/3, −y+2/3, −z+2/3; (xxxiii) y−2/3, y−x−1/3, −z+2/3; (xxxiv) y−2/3, y−x+2/3, −z+2/3; (xxxv) y+1/3, y−x+2/3, −z+2/3; (xxxvi) x−y−2/3, x−1/3, −z+2/3; (xxxvii) x−y−2/3, x+2/3, −z+2/3; (xxxviii) x−y+1/3, x+2/3, −z+2/3; (xxxix) x−y−2/3, −y−1/3, −z+2/3; (xl) x−y−2/3, −y+2/3, −z+2/3; (xli) x−y+1/3, −y+2/3, −z+2/3; (xlii) y−2/3, x−1/3, −z+2/3; (xliii) y−2/3, x+2/3, −z+2/3; (xliv) y+1/3, x+2/3, −z+2/3; (xlv) −x−2/3, y−x−1/3, −z+2/3; (xlvi) −x−2/3, y−x+2/3, −z+2/3; (xlvii) −x+1/3, y−x+2/3, −z+2/3; (xlviii) x−1/3, y−2/3, z+1/3; (xlix) x−1/3, y+1/3, z+1/3; (l) x+2/3, y+1/3, z+1/3; (li) −x−1/3, −y−2/3, −z+1/3; (lii) −x+2/3, −y−2/3, −z+1/3; (liii) −x+2/3, −y+1/3, −z+1/3; (liv) y−1/3, y−x−2/3, −z+1/3; (lv) y+2/3, y−x−2/3, −z+1/3; (lvi) x−y+2/3, x−2/3, −z+1/3; (lvii) x−y+2/3, x+1/3, −z+1/3; (lviii) x−y+2/3, −y−2/3, −z+1/3; (lix) x−y+2/3, −y+1/3, −z+1/3; (lx) y−1/3, x−2/3, −z+1/3; (lxi) y+2/3, x+1/3, −z+1/3; (lxii) −x−1/3, y−x−2/3, −z+1/3; (lxiii) −x+2/3, y−x−2/3, −z+1/3; (lxiv) y+2/3, y−x+1/3, −z+1/3; (lxv) x−y−1/3, x−2/3, −z+1/3; (lxvi) x−y−1/3, −y−2/3, −z+1/3; (lxvii) y+2/3, x−2/3, −z+1/3; (lxviii) −x+2/3, y−x+1/3, −z+1/3; (lxix) −y−1/3, x−y+1/3, z+1/3; (lxx) −y+2/3, x−y+1/3, z+1/3; (lxxi) y−x−1/3, −x−2/3, z+1/3; (lxxii) y−x−1/3, −x+1/3, z+1/3; (lxxiii) y−x−1/3, y−2/3, z+1/3; (lxxiv) y−x−1/3, y+1/3, z+1/3; (lxxv) −y−1/3, −x−2/3, z+1/3; (lxxvi) −y+2/3, −x+1/3, z+1/3; (lxxvii) x−1/3, x−y+1/3, z+1/3; (lxxviii) x+2/3, x−y+1/3, z+1/3; (lxxix) −x, −y, −z+1; (lxxx) y, y−x, −z+1; (lxxxi) x−y, x, −z+1; (lxxxii) x−y, −y, −z+1; (lxxxiii) y, x, −z+1; (lxxxiv) −x, y−x, −z+1; (lxxxv) −y−1/3, −x+1/3, z+1/3; (lxxxvi) −y, x−y+1, z; (lxxxvii) y−x−1, −x, z; (lxxxviii) y−x−1, y, z; (lxxxix) x, x−y+1, z.

(S3P4X0_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8974 (6) Å	T = 298 K
c = 2.8297 (9) Å	Particle morphology: Pressure cell anvil material
V = 20.57 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.881 < d < 2.998 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.040	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 60.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.02 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 123.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 248.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.032	36 parameters
Rexp = 0.023	0 restraints
R(F^2) = 0.17019	(Δ/σ)max = 0.01
χ^2 = 1.932	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 2.23627 2: -0.566994 3: 0.896526 4: -0.182112 5: 0.350911 6: -0.196381 7: 0.201360 8: -0.135196 9: 0.125708 10: -9.856300E-0211: 5.324140E-0212: -2.400480E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.80545 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.188 (3)	P—Pb2	3.313 (2)
Pb1—Pb2^i	4.188 (3)	P—Pb2	3.396 (19)
Pb1—Pb2^ii	4.188 (3)	P—Pb2	3.396 (19)
Pb1—Pb2^iii	4.188 (3)	P—Pb2	3.228 (19)
Pb1—Pb2^iv	4.188 (3)	P—Pb2	3.313 (2)
Pb1—Pb2^v	4.188 (3)	P—Pb2	3.396 (19)
Pb1—Pb2	4.188 (3)	P—Pb2	3.313 (2)
Pb1—Pb2	4.188 (3)	P—Pb2	3.228 (19)
Pb1—Pb2	4.188 (3)	P—Pb2	3.228 (19)
Pb1—Pb2	4.188 (3)	P—Pb2	3.396 (19)
Pb1—Pb2	4.188 (3)	P—Pb2	3.313 (2)
Pb1—Pb2	4.188 (3)	P—Pb2	3.313 (2)
Pb1—Pb2	3.993 (2)	P—Pb2	3.228 (19)
Pb1—Pb2	3.922 (16)	P—Pb2	3.396 (19)
Pb1—Pb2	4.062 (16)	P—Pb2	4.128 (16)
Pb1—Pb2	4.062 (16)	P—Pb2	4.195 (5)
Pb1—Pb2	3.993 (2)	P—Pb2	4.195 (5)
Pb1—Pb2	3.922 (16)	P—Pb2	4.128 (16)
Pb1—Pb2	3.922 (16)	P—Pb2	4.195 (5)
Pb1—Pb2	4.062 (16)	P—Pb2	4.128 (16)
Pb1—Pb2	3.993 (2)	P—Pb2	4.128 (16)
Pb1—Pb2	3.922 (16)	P—Pb2	4.195 (5)
Pb1—Pb2	3.993 (2)	P—Pb2	4.195 (5)
Pb1—Pb2	4.062 (16)	P—Pb2	4.128 (16)
Pb1—Pb2	4.062 (16)	P—Pb2	4.128 (16)
Pb1—Pb2	3.922 (16)	P—Pb2	4.195 (5)
Pb1—Pb2	3.993 (2)	P—P	3.867 (13)
Pb1—Pb2	3.993 (2)	P—P	4.197 (9)
Pb1—Pb2	4.062 (16)	P—P	4.197 (9)
Pb1—Pb2	3.922 (16)	P—P	4.197 (9)
Pb1—Pb2	4.062 (16)	P—O1	1.491 (9)
Pb1—Pb2	3.922 (16)	P—O1	3.392 (3)
Pb1—Pb2	3.993 (2)	P—O1	3.392 (3)
Pb1—Pb2	3.922 (16)	P—O1	3.392 (3)
Pb1—Pb2	3.993 (2)	P—O2	1.546 (4)
Pb1—Pb2	4.062 (16)	P—O2^i	1.546 (4)
Pb1—Pb2	3.993 (2)	P—O2^ii	1.546 (4)
Pb1—Pb2	4.062 (16)	P—O2^iii	1.546 (4)
Pb1—Pb2	3.922 (16)	P—O2^iv	1.546 (4)
Pb1—Pb2	4.062 (16)	P—O2^v	1.546 (4)
Pb1—Pb2	3.993 (2)	P—O2	3.643 (7)
Pb1—Pb2	3.922 (16)	P—O2	3.643 (7)
Pb1—Pb2	3.993 (2)	P—O2	3.643 (7)
Pb1—Pb2	3.922 (16)	P—O2	3.643 (7)
Pb1—Pb2	4.062 (16)	P—O2	3.643 (7)
Pb1—Pb2	3.922 (16)	P—O2	3.643 (7)
Pb1—Pb2	4.062 (16)	O1—Pb1	3.1327 (2)
Pb1—Pb2	3.993 (2)	O1—Pb1	3.1327 (2)
Pb1—P	3.429 (3)	O1—Pb1	3.1327 (2)
Pb1—P	3.429 (3)	O1—Pb2	2.383 (6)
Pb1—P	3.429 (3)	O1—Pb2^i	2.383 (6)
Pb1—P	3.429 (3)	O1—Pb2^ii	2.383 (6)
Pb1—P	3.429 (3)	O1—Pb2^iii	2.383 (6)
Pb1—P	3.429 (3)	O1—Pb2^iv	2.383 (6)
Pb1—O1	3.1327 (2)	O1—Pb2^v	2.383 (6)
Pb1—O1	3.1327 (2)	O1—Pb2	4.051 (4)
Pb1—O1	3.1327 (2)	O1—Pb2	4.120 (17)
Pb1—O1	3.1327 (2)	O1—Pb2	3.982 (15)
Pb1—O1	3.1327 (2)	O1—Pb2	3.982 (15)
Pb1—O1	3.1327 (2)	O1—Pb2	4.051 (4)
Pb1—O2	2.555 (3)	O1—Pb2	4.120 (17)
Pb1—O2	2.555 (3)	O1—Pb2	4.120 (17)
Pb1—O2	2.555 (3)	O1—Pb2	3.982 (15)
Pb1—O2	2.555 (3)	O1—Pb2	4.051 (4)
Pb1—O2	2.555 (3)	O1—Pb2	4.120 (17)
Pb1—O2	2.555 (3)	O1—Pb2	4.051 (4)
Pb1—O2	2.555 (3)	O1—Pb2	3.982 (15)
Pb1—O2	2.555 (3)	O1—Pb2	3.982 (15)
Pb1—O2	2.555 (3)	O1—Pb2	4.120 (17)
Pb1—O2	2.555 (3)	O1—Pb2	4.051 (4)
Pb1—O2	2.555 (3)	O1—Pb2	4.051 (4)
Pb1—O2	2.555 (3)	O1—Pb2	3.982 (15)
Pb2—Pb1	4.188 (3)	O1—Pb2	4.120 (17)
Pb2—Pb1	4.062 (16)	O1—P	1.491 (9)
Pb2—Pb1	3.922 (16)	O1—P	3.392 (3)
Pb2—Pb1	3.993 (2)	O1—P	3.392 (3)
Pb2—Pb2^i	0.18 (4)	O1—P	3.392 (3)
Pb2—Pb2^ii	0.18 (4)	O1—O1	3.1369 (6)
Pb2—Pb2^iii	0.10 (2)	O1—O1	3.1369 (6)
Pb2—Pb2^iv	0.10 (2)	O1—O1	3.1369 (6)
Pb2—Pb2^v	0.21 (5)	O1—O2	2.487 (5)
Pb2—Pb2	3.73 (4)	O1—O2^i	2.487 (5)
Pb2—Pb2	3.42 (3)	O1—O2^ii	2.487 (5)
Pb2—Pb2	3.575 (4)	O1—O2^iii	2.487 (5)
Pb2—Pb2	3.571 (3)	O1—O2^iv	2.487 (5)
Pb2—Pb2	3.491 (17)	O1—O2^v	2.487 (5)
Pb2—Pb2	3.648 (19)	O1—O2	3.328 (13)
Pb2—Pb2	3.648 (19)	O1—O2	3.220 (14)
Pb2—Pb2	3.571 (3)	O1—O2	3.220 (14)
Pb2—Pb2	3.491 (17)	O1—O2	3.328 (13)
Pb2—Pb2	3.73 (4)	O1—O2	3.220 (14)
Pb2—Pb2	3.494 (16)	O1—O2	3.328 (13)
Pb2—Pb2	3.494 (16)	O1—O2	3.328 (13)
Pb2—Pb2	3.65 (2)	O1—O2	3.220 (14)
Pb2—Pb2	3.41 (4)	O1—O2	3.220 (14)
Pb2—Pb2	3.65 (2)	O1—O2	3.328 (13)
Pb2—Pb2	3.569 (3)	O1—O2	3.328 (13)
Pb2—Pb2	3.569 (3)	O1—O2	3.220 (14)
Pb2—Pb2	3.569 (3)	O2—Pb1	2.555 (3)
Pb2—P	3.874 (8)	O2—Pb2	2.882 (18)
Pb2—P	4.195 (5)	O2—Pb2	2.653 (19)
Pb2—P	4.128 (16)	O2—Pb2	2.73 (3)
Pb2—P	3.313 (2)	O2—Pb2	2.81 (3)
Pb2—P	3.396 (19)	O2—Pb2	2.889 (19)
Pb2—P	3.228 (19)	O2—Pb2	2.661 (18)
Pb2—O1	2.383 (6)	O2—Pb2	2.94 (3)
Pb2—O1	4.051 (4)	O2—Pb2	2.61 (3)
Pb2—O1	4.120 (17)	O2—Pb2	2.78 (2)
Pb2—O1	3.982 (15)	O2—Pb2	2.75 (2)
Pb2—O2	2.872 (12)	O2—Pb2	2.788 (19)
Pb2—O2	2.766 (13)	O2—Pb2	2.76 (2)
Pb2—O2	2.823 (4)	O2—Pb2	2.872 (12)
Pb2—O2	2.818 (4)	O2—Pb2	2.823 (4)
Pb2—O2	2.875 (12)	O2—Pb2	2.766 (13)
Pb2—O2	2.768 (13)	O2—Pb2	2.818 (4)
Pb2—O2	2.882 (18)	O2—Pb2	2.875 (12)
Pb2—O2	2.653 (19)	O2—Pb2	2.768 (13)
Pb2—O2	2.661 (18)	O2—P	1.546 (4)
Pb2—O2	2.889 (19)	O2—P	3.643 (7)
Pb2—O2	2.81 (3)	O2—O1	2.487 (5)
Pb2—O2	2.73 (3)	O2—O1	3.328 (13)
Pb2—O2	2.94 (3)	O2—O1	3.220 (14)
Pb2—O2	2.61 (3)	O2—O2^i	2.517 (6)
Pb2—O2	2.75 (2)	O2—O2^vi	2.911 (6)
Pb2—O2	2.78 (2)	O2—O2^vii	2.911 (6)
Pb2—O2	2.788 (19)	O2—O2^ii	2.517 (6)
Pb2—O2	2.76 (2)	O2—O2^viii	2.974 (17)
P—Pb1	3.429 (3)	O2—O2^iii	2.449 (17)
P—Pb1	3.429 (3)	O2—O2^iv	0.13 (3)
P—Pb1	3.429 (3)	O2—O2^v	2.580 (17)
P—Pb2	3.874 (8)	O2—O2^ix	2.844 (17)
P—Pb2^i	3.874 (8)	O2—O2	4.045 (7)
P—Pb2^ii	3.874 (8)	O2—O2	3.167 (5)
P—Pb2^iii	3.874 (8)	O2—O2	3.167 (5)
P—Pb2^iv	3.874 (8)	O2—O2	3.219 (15)
P—Pb2^v	3.874 (8)	O2—O2	4.043 (7)
P—Pb2	3.313 (2)	O2—O2	3.116 (13)
P—Pb2	3.396 (19)	O2—O2	4.199 (6)
P—Pb2	3.228 (19)	O2—O2	4.199 (6)
P—Pb2	3.228 (19)	O2—O2	4.155 (12)
O1—P—O2	109.9 (3)	O2^i—P—O2^ii	109.0 (3)
O1—P—O2^i	109.9 (3)	O2^i—P—O2^iii	113.1 (10)
O1—P—O2^ii	109.9 (3)	O2^i—P—O2^iv	104.8 (10)
O1—P—O2^iii	109.9 (3)	O2^i—P—O2^v	4.8 (12)
O1—P—O2^iv	109.9 (3)	O2^ii—P—O2^iii	4.8 (12)
O1—P—O2^v	109.9 (3)	O2^ii—P—O2^iv	113.1 (10)
O2—P—O2^i	109.0 (3)	O2^ii—P—O2^v	104.8 (10)
O2—P—O2^ii	109.0 (3)	O2^iii—P—O2^iv	109.0 (3)
O2—P—O2^iii	104.8 (10)	O2^iii—P—O2^v	109.0 (3)
O2—P—O2^iv	4.8 (12)	O2^iv—P—O2^v	109.0 (3)
O2—P—O2^v	113.1 (10)	P—O2—O2^iv	87.6 (6)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) x, y, −z; (iv) y−x, −x, z; (v) −y, x−y, −z; (vi) y−x, −x+1, −z; (vii) −y−1, x−y, z; (viii) x−1, y, −z; (ix) −y, x−y+1, −z.

(S3P4X0_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5347 (7) Å	Particle morphology: Component of pressure cell, not sample
V = 44.16 (3) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.881 < d < 2.998 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.040	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 60.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.02 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 123.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 248.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.032	36 parameters
Rexp = 0.023	0 restraints
R(F^2) = 0.17019	(Δ/σ)max = 0.01
χ^2 = 1.932	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 2.23627 2: -0.566994 3: 0.896526 4: -0.182112 5: 0.350911 6: -0.196381 7: 0.201360 8: -0.135196 9: 0.125708 10: -9.856300E-0211: 5.324140E-0212: -2.400480E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.80545 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.188 (3)	P—Pb2^lv	3.313 (2)
Pb1—Pb2^i	4.188 (3)	P—Pb2^lxiv	3.396 (19)
Pb1—Pb2^ii	4.188 (3)	P—Pb2^lxv	3.396 (19)
Pb1—Pb2^iii	4.188 (3)	P—Pb2^lvi	3.228 (19)
Pb1—Pb2^iv	4.188 (3)	P—Pb2^lvii	3.313 (2)
Pb1—Pb2^v	4.188 (3)	P—Pb2^lxvi	3.396 (19)
Pb1—Pb2^vi	4.188 (3)	P—Pb2^lviii	3.313 (2)
Pb1—Pb2^vii	4.188 (3)	P—Pb2^lix	3.228 (19)
Pb1—Pb2^viii	4.188 (3)	P—Pb2^lx	3.228 (19)
Pb1—Pb2^ix	4.188 (3)	P—Pb2^lxvii	3.396 (19)
Pb1—Pb2^x	4.188 (3)	P—Pb2^lxi	3.313 (2)
Pb1—Pb2^xi	4.188 (3)	P—Pb2^lxii	3.313 (2)
Pb1—Pb2^xii	3.993 (2)	P—Pb2^lxiii	3.228 (19)
Pb1—Pb2^xiii	3.922 (16)	P—Pb2^lxviii	3.396 (19)
Pb1—Pb2^xiv	4.062 (16)	P—Pb2^xlviii	4.128 (16)
Pb1—Pb2^xv	4.062 (16)	P—Pb2^l	4.195 (5)
Pb1—Pb2^xvi	3.993 (2)	P—Pb2^lxix	4.195 (5)
Pb1—Pb2^xvii	3.922 (16)	P—Pb2^lxx	4.128 (16)
Pb1—Pb2^xviii	3.922 (16)	P—Pb2^lxxi	4.195 (5)
Pb1—Pb2^xix	4.062 (16)	P—Pb2^lxxii	4.128 (16)
Pb1—Pb2^xx	3.993 (2)	P—Pb2^lxxiii	4.128 (16)
Pb1—Pb2^xxi	3.922 (16)	P—Pb2^lxxiv	4.195 (5)
Pb1—Pb2^xxii	3.993 (2)	P—Pb2^lxxv	4.195 (5)
Pb1—Pb2^xxiii	4.062 (16)	P—Pb2^lxxvi	4.128 (16)
Pb1—Pb2^xxiv	4.062 (16)	P—Pb2^lxxvii	4.128 (16)
Pb1—Pb2^xxv	3.922 (16)	P—Pb2^lxxviii	4.195 (5)
Pb1—Pb2^xxvi	3.993 (2)	P—P^lxxix	3.867 (13)
Pb1—Pb2^xxvii	3.993 (2)	P—P^li	4.197 (9)
Pb1—Pb2^xxviii	4.062 (16)	P—P^lii	4.197 (9)
Pb1—Pb2^xxix	3.922 (16)	P—P^liii	4.197 (9)
Pb1—Pb2^xxx	4.062 (16)	P—O1	1.491 (9)
Pb1—Pb2^xxxi	3.922 (16)	P—O1^li	3.392 (3)
Pb1—Pb2^xxxii	3.993 (2)	P—O1^lii	3.392 (3)
Pb1—Pb2^xxxiii	3.922 (16)	P—O1^liii	3.392 (3)
Pb1—Pb2^xxxiv	3.993 (2)	P—O2	1.546 (4)
Pb1—Pb2^xxxv	4.062 (16)	P—O2^i	1.546 (4)
Pb1—Pb2^xxxvi	3.993 (2)	P—O2^ii	1.546 (4)
Pb1—Pb2^xxxvii	4.062 (16)	P—O2^iii	1.546 (4)
Pb1—Pb2^xxxviii	3.922 (16)	P—O2^iv	1.546 (4)
Pb1—Pb2^xxxix	4.062 (16)	P—O2^v	1.546 (4)
Pb1—Pb2^xl	3.993 (2)	P—O2^lxxix	3.643 (7)
Pb1—Pb2^xli	3.922 (16)	P—O2^lxxx	3.643 (7)
Pb1—Pb2^xlii	3.993 (2)	P—O2^lxxxi	3.643 (7)
Pb1—Pb2^xliii	3.922 (16)	P—O2^lxxxii	3.643 (7)
Pb1—Pb2^xliv	4.062 (16)	P—O2^lxxxiii	3.643 (7)
Pb1—Pb2^xlv	3.922 (16)	P—O2^lxxxiv	3.643 (7)
Pb1—Pb2^xlvi	4.062 (16)	O1—Pb1^xlviii	3.1327 (2)
Pb1—Pb2^xlvii	3.993 (2)	O1—Pb1^xlix	3.1327 (2)
Pb1—P^xii	3.429 (3)	O1—Pb1^l	3.1327 (2)
Pb1—P^xiii	3.429 (3)	O1—Pb2	2.383 (6)
Pb1—P^xiv	3.429 (3)	O1—Pb2^i	2.383 (6)
Pb1—P^xxx	3.429 (3)	O1—Pb2^ii	2.383 (6)
Pb1—P^xxxi	3.429 (3)	O1—Pb2^iii	2.383 (6)
Pb1—P^xxxii	3.429 (3)	O1—Pb2^iv	2.383 (6)
Pb1—O1^xii	3.1327 (2)	O1—Pb2^v	2.383 (6)
Pb1—O1^xiii	3.1327 (2)	O1—Pb2^li	4.051 (4)
Pb1—O1^xiv	3.1327 (2)	O1—Pb2^lii	4.120 (17)
Pb1—O1^xxx	3.1327 (2)	O1—Pb2^liii	3.982 (15)
Pb1—O1^xxxi	3.1327 (2)	O1—Pb2^liv	3.982 (15)
Pb1—O1^xxxii	3.1327 (2)	O1—Pb2^lv	4.051 (4)
Pb1—O2^xiii	2.555 (3)	O1—Pb2^lxiv	4.120 (17)
Pb1—O2^xvii	2.555 (3)	O1—Pb2^lxv	4.120 (17)
Pb1—O2^xviii	2.555 (3)	O1—Pb2^lvi	3.982 (15)
Pb1—O2^xxi	2.555 (3)	O1—Pb2^lvii	4.051 (4)
Pb1—O2^xxv	2.555 (3)	O1—Pb2^lxvi	4.120 (17)
Pb1—O2^xxix	2.555 (3)	O1—Pb2^lviii	4.051 (4)
Pb1—O2^xxxi	2.555 (3)	O1—Pb2^lix	3.982 (15)
Pb1—O2^xxxiii	2.555 (3)	O1—Pb2^lx	3.982 (15)
Pb1—O2^xxxviii	2.555 (3)	O1—Pb2^lxvii	4.120 (17)
Pb1—O2^xli	2.555 (3)	O1—Pb2^lxi	4.051 (4)
Pb1—O2^xliii	2.555 (3)	O1—Pb2^lxii	4.051 (4)
Pb1—O2^xlv	2.555 (3)	O1—Pb2^lxiii	3.982 (15)
Pb2—Pb1	4.188 (3)	O1—Pb2^lxviii	4.120 (17)
Pb2—Pb1^xlviii	4.062 (16)	O1—P	1.491 (9)
Pb2—Pb1^xlix	3.922 (16)	O1—P^li	3.392 (3)
Pb2—Pb1^l	3.993 (2)	O1—P^lii	3.392 (3)
Pb2—Pb2^i	0.18 (4)	O1—P^liii	3.392 (3)
Pb2—Pb2^ii	0.18 (4)	O1—O1^li	3.1369 (6)
Pb2—Pb2^iii	0.10 (2)	O1—O1^lii	3.1369 (6)
Pb2—Pb2^iv	0.10 (2)	O1—O1^liii	3.1369 (6)
Pb2—Pb2^v	0.21 (5)	O1—O2	2.487 (5)
Pb2—Pb2^xxx	3.73 (4)	O1—O2^i	2.487 (5)
Pb2—Pb2^xxxi	3.42 (3)	O1—O2^ii	2.487 (5)
Pb2—Pb2^xxxii	3.575 (4)	O1—O2^iii	2.487 (5)
Pb2—Pb2^xxxiii	3.571 (3)	O1—O2^iv	2.487 (5)
Pb2—Pb2^xxxiv	3.491 (17)	O1—O2^v	2.487 (5)
Pb2—Pb2^xxxv	3.648 (19)	O1—O2^li	3.328 (13)
Pb2—Pb2^xxxvi	3.648 (19)	O1—O2^liii	3.220 (14)
Pb2—Pb2^xxxvii	3.571 (3)	O1—O2^liv	3.220 (14)
Pb2—Pb2^xxxviii	3.491 (17)	O1—O2^lv	3.328 (13)
Pb2—Pb2^xxxix	3.73 (4)	O1—O2^lvi	3.220 (14)
Pb2—Pb2^xl	3.494 (16)	O1—O2^lvii	3.328 (13)
Pb2—Pb2^xli	3.494 (16)	O1—O2^lviii	3.328 (13)
Pb2—Pb2^xlii	3.65 (2)	O1—O2^lix	3.220 (14)
Pb2—Pb2^xliii	3.41 (4)	O1—O2^lx	3.220 (14)
Pb2—Pb2^xliv	3.65 (2)	O1—O2^lxi	3.328 (13)
Pb2—Pb2^xlv	3.569 (3)	O1—O2^lxii	3.328 (13)
Pb2—Pb2^xlvi	3.569 (3)	O1—O2^lxiii	3.220 (14)
Pb2—Pb2^xlvii	3.569 (3)	O2—Pb1^xlix	2.555 (3)
Pb2—P	3.874 (8)	O2—Pb2^li	2.882 (18)
Pb2—P^xii	4.195 (5)	O2—Pb2^liii	2.653 (19)
Pb2—P^xiv	4.128 (16)	O2—Pb2^liv	2.73 (3)
Pb2—P^li	3.313 (2)	O2—Pb2^lxiv	2.81 (3)
Pb2—P^lii	3.396 (19)	O2—Pb2^lxv	2.889 (19)
Pb2—P^liii	3.228 (19)	O2—Pb2^lvii	2.661 (18)
Pb2—O1	2.383 (6)	O2—Pb2^lxvi	2.94 (3)
Pb2—O1^li	4.051 (4)	O2—Pb2^lix	2.61 (3)
Pb2—O1^lii	4.120 (17)	O2—Pb2^lx	2.78 (2)
Pb2—O1^liii	3.982 (15)	O2—Pb2^lxi	2.75 (2)
Pb2—O2^xiii	2.872 (12)	O2—Pb2^lxii	2.788 (19)
Pb2—O2^xvii	2.766 (13)	O2—Pb2^lxviii	2.76 (2)
Pb2—O2^xviii	2.823 (4)	O2—Pb2^xlix	2.872 (12)
Pb2—O2^xxi	2.818 (4)	O2—Pb2^lxix	2.823 (4)
Pb2—O2^xxv	2.875 (12)	O2—Pb2^lxxii	2.766 (13)
Pb2—O2^xxix	2.768 (13)	O2—Pb2^lxxiv	2.818 (4)
Pb2—O2^li	2.882 (18)	O2—Pb2^lxxxv	2.875 (12)
Pb2—O2^liii	2.653 (19)	O2—Pb2^lxxvii	2.768 (13)
Pb2—O2^liv	2.661 (18)	O2—P	1.546 (4)
Pb2—O2^lv	2.889 (19)	O2—P^lxxix	3.643 (7)
Pb2—O2^lvi	2.81 (3)	O2—O1	2.487 (5)
Pb2—O2^lvii	2.73 (3)	O2—O1^li	3.328 (13)
Pb2—O2^lviii	2.94 (3)	O2—O1^liii	3.220 (14)
Pb2—O2^lix	2.61 (3)	O2—O2^i	2.517 (6)
Pb2—O2^lx	2.75 (2)	O2—O2^lxxxvi	2.911 (6)
Pb2—O2^lxi	2.78 (2)	O2—O2^lxxxvii	2.911 (6)
Pb2—O2^lxii	2.788 (19)	O2—O2^ii	2.517 (6)
Pb2—O2^lxiii	2.76 (2)	O2—O2^lxxxviii	2.974 (17)
P—Pb1^xlviii	3.429 (3)	O2—O2^iii	2.449 (17)
P—Pb1^xlix	3.429 (3)	O2—O2^iv	0.13 (3)
P—Pb1^l	3.429 (3)	O2—O2^v	2.580 (17)
P—Pb2	3.874 (8)	O2—O2^lxxxix	2.844 (17)
P—Pb2^i	3.874 (8)	O2—O2^lxxix	4.045 (7)
P—Pb2^ii	3.874 (8)	O2—O2^lxxx	3.167 (5)
P—Pb2^iii	3.874 (8)	O2—O2^lxxxi	3.167 (5)
P—Pb2^iv	3.874 (8)	O2—O2^lxxxii	3.219 (15)
P—Pb2^v	3.874 (8)	O2—O2^lxxxiii	4.043 (7)
P—Pb2^li	3.313 (2)	O2—O2^lxxxiv	3.116 (13)
P—Pb2^lii	3.396 (19)	O2—O2^liv	4.199 (6)
P—Pb2^liii	3.228 (19)	O2—O2^lvii	4.199 (6)
P—Pb2^liv	3.228 (19)	O2—O2^lix	4.155 (12)
O1—P—O2	109.9 (3)	O2^i—P—O2^ii	109.0 (3)
O1—P—O2^i	109.9 (3)	O2^i—P—O2^iii	113.1 (10)
O1—P—O2^ii	109.9 (3)	O2^i—P—O2^iv	104.8 (10)
O1—P—O2^iii	109.9 (3)	O2^i—P—O2^v	4.8 (12)
O1—P—O2^iv	109.9 (3)	O2^ii—P—O2^iii	4.8 (12)
O1—P—O2^v	109.9 (3)	O2^ii—P—O2^iv	113.1 (10)
O2—P—O2^i	109.0 (3)	O2^ii—P—O2^v	104.8 (10)
O2—P—O2^ii	109.0 (3)	O2^iii—P—O2^iv	109.0 (3)
O2—P—O2^iii	104.8 (10)	O2^iii—P—O2^v	109.0 (3)
O2—P—O2^iv	4.8 (12)	O2^iv—P—O2^v	109.0 (3)
O2—P—O2^v	113.1 (10)	P—O2—O2^iv	87.6 (6)

Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) x, y, −z; (iv) −z, x, y; (v) y, −z, x; (vi) −x, −y, −z; (vii) −z, −x, −y; (viii) −y, −z, −x; (ix) −x, −y, z; (x) z, −x, −y; (xi) −y, z, −x; (xii) x−1, y−1/2, z−1/2; (xiii) x, y−1/2, z−1/2; (xiv) x, y+1/2, z−1/2; (xv) z−1, x−1/2, y−1/2; (xvi) z, x−1/2, y−1/2; (xvii) z, x+1/2, y−1/2; (xviii) y−1, z−1/2, x−1/2; (xix) y, z−1/2, x−1/2; (xx) y, z+1/2, x−1/2; (xxi) x−1, y−1/2, −z−1/2; (xxii) x, y−1/2, −z−1/2; (xxiii) x, y+1/2, −z−1/2; (xxiv) −z−1, x−1/2, y−1/2; (xxv) −z, x−1/2, y−1/2; (xxvi) −z, x+1/2, y−1/2; (xxvii) y−1, −z−1/2, x−1/2; (xxviii) y, −z−1/2, x−1/2; (xxix) y, −z+1/2, x−1/2; (xxx) −x−1/2, −y−1, −z+1/2; (xxxi) −x−1/2, −y, −z+1/2; (xxxii) −x+1/2, −y, −z+1/2; (xxxiii) −z−1/2, −x−1, −y+1/2; (xxxiv) −z−1/2, −x, −y+1/2; (xxxv) −z+1/2, −x, −y+1/2; (xxxvi) −y−1/2, −z−1, −x+1/2; (xxxvii) −y−1/2, −z, −x+1/2; (xxxviii) −y+1/2, −z, −x+1/2; (xxxix) −x−1/2, −y−1, z+1/2; (xl) −x−1/2, −y, z+1/2; (xli) −x+1/2, −y, z+1/2; (xlii) z−1/2, −x−1, −y+1/2; (xliii) z−1/2, −x, −y+1/2; (xliv) z+1/2, −x, −y+1/2; (xlv) −y−1/2, z−1, −x+1/2; (xlvi) −y−1/2, z, −x+1/2; (xlvii) −y+1/2, z, −x+1/2; (xlviii) x−1/2, y−1, z+1/2; (xlix) x−1/2, y, z+1/2; (l) x+1/2, y, z+1/2; (li) −x−1, −y−1/2, −z+1/2; (lii) −x, −y−1/2, −z+1/2; (liii) −x, −y+1/2, −z+1/2; (liv) −z−1, −x−1/2, −y+1/2; (lv) −z, −x−1/2, −y+1/2; (lvi) −y, −z−1/2, −x+1/2; (lvii) −y, −z+1/2, −x+1/2; (lviii) −x, −y−1/2, z+1/2; (lix) −x, −y+1/2, z+1/2; (lx) z−1, −x−1/2, −y+1/2; (lxi) z, −x+1/2, −y+1/2; (lxii) −y−1, z−1/2, −x+1/2; (lxiii) −y, z−1/2, −x+1/2; (lxiv) −z, −x+1/2, −y+1/2; (lxv) −y−1, −z−1/2, −x+1/2; (lxvi) −x−1, −y−1/2, z+1/2; (lxvii) z, −x−1/2, −y+1/2; (lxviii) −y, z+1/2, −x+1/2; (lxix) z−1/2, x, y+1/2; (lxx) z+1/2, x, y+1/2; (lxxi) y−1/2, z−1, x+1/2; (lxxii) y−1/2, z, x+1/2; (lxxiii) x−1/2, y−1, −z+1/2; (lxxiv) x−1/2, y, −z+1/2; (lxxv) −z−1/2, x−1, y+1/2; (lxxvi) −z+1/2, x, y+1/2; (lxxvii) y−1/2, −z, x+1/2; (lxxviii) y+1/2, −z, x+1/2; (lxxix) −x, −y, −z+1; (lxxx) −z, −x, −y+1; (lxxxi) −y, −z, −x+1; (lxxxii) −x, −y, z+1; (lxxxiii) z, −x, −y+1; (lxxxiv) −y, z, −x+1; (lxxxv) −z−1/2, x, y+1/2; (lxxxvi) z, x+1, y; (lxxxvii) y−1, z, x; (lxxxviii) x−1, y, −z; (lxxxix) y, −z+1, x.

(S3P5T_phase_1)

Crystal data

O8P2Pb3	Z = 3
Mr = 811.74	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.3925 (3) Å	Particle morphology: plate
c = 19.9080 (15) Å	irregular, 6 × 6 mm
V = 501.34 (5) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.881 < d < 2.998 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.058	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 64.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.97 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 167.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.043	34 parameters
Rexp = 0.036	0 restraints
R(F^2) = 0.17381	(Δ/σ)max = 0.01
χ^2 = 1.513	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.29615 2: -0.262129 3: 0.585253 4: -9.040860E-02 5: 0.279121 6: -0.111587 7: 0.157996 8: -6.275300E-02 9: 8.944730E-0210: -4.246060E-0211: 3.246880E-0212: -4.863080E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.78149 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.0	0.0	0.0	0.0210 (14)*
Pb2	0.0	0.0	0.2086 (2)	0.0210 (14)*
P	0.0	0.0	0.4047 (5)	0.0126 (18)*
O1	0.0	0.0	0.3282 (3)	0.0175 (12)*
O2	−0.1549 (5)	0.1549 (5)	0.4304 (2)	0.0175 (12)*

Geometric parameters (Å, º)

Pb1—Pb2	4.152 (4)	P—Pb2^xv	3.290 (3)
Pb1—Pb2^i	4.152 (4)	P—Pb2^xvi	3.290 (3)
Pb1—Pb2^ii	3.983 (3)	P—Pb2^xvii	3.290 (3)
Pb1—Pb2^iii	3.983 (3)	P—Pb2^xii	4.142 (8)
Pb1—Pb2^iv	3.983 (3)	P—Pb2^xiii	4.142 (8)
Pb1—Pb2^v	3.983 (3)	P—Pb2^xiv	4.142 (8)
Pb1—Pb2^vi	3.983 (3)	P—P^xxii	3.795 (18)
Pb1—Pb2^vii	3.983 (3)	P—O1	1.524 (11)
Pb1—P^ii	3.422 (4)	P—O1^xv	3.381 (4)
Pb1—P^iii	3.422 (4)	P—O1^xvi	3.381 (4)
Pb1—P^iv	3.422 (4)	P—O1^xvii	3.381 (4)
Pb1—P^v	3.422 (4)	P—O2	1.535 (6)
Pb1—P^vi	3.422 (4)	P—O2^xxiii	1.535 (6)
Pb1—P^vii	3.422 (4)	P—O2^xxiv	1.535 (6)
Pb1—O1^ii	3.1151 (3)	P—O2^xxii	3.587 (10)
Pb1—O1^iii	3.1151 (3)	P—O2^xxv	3.587 (10)
Pb1—O1^iv	3.1151 (3)	P—O2^xxvi	3.587 (10)
Pb1—O1^v	3.1151 (3)	O1—Pb1^xii	3.1151 (3)
Pb1—O1^vi	3.1151 (3)	O1—Pb1^xiii	3.1151 (3)
Pb1—O1^vii	3.1151 (3)	O1—Pb1^xiv	3.1151 (3)
Pb1—O2^iii	2.552 (4)	O1—Pb2	2.381 (8)
Pb1—O2^viii	2.552 (4)	O1—Pb2^xv	4.048 (5)
Pb1—O2^ix	2.552 (4)	O1—Pb2^xvi	4.048 (5)
Pb1—O2^vi	2.552 (4)	O1—Pb2^xvii	4.048 (5)
Pb1—O2^x	2.552 (4)	O1—P	1.524 (11)
Pb1—O2^xi	2.552 (4)	O1—P^xv	3.381 (4)
Pb2—Pb1	4.152 (4)	O1—P^xvi	3.381 (4)
Pb2—Pb1^xii	3.983 (3)	O1—P^xvii	3.381 (4)
Pb2—Pb1^xiii	3.983 (3)	O1—O1^xv	3.1202 (9)
Pb2—Pb1^xiv	3.983 (3)	O1—O1^xvi	3.1202 (9)
Pb2—Pb2^v	3.532 (4)	O1—O1^xvii	3.1202 (9)
Pb2—Pb2^vi	3.532 (4)	O1—O2	2.498 (7)
Pb2—Pb2^vii	3.532 (4)	O1—O2^xxiii	2.498 (7)
Pb2—P	3.904 (11)	O1—O2^xxiv	2.498 (7)
Pb2—P^ii	4.142 (8)	O1—O2^xv	3.260 (4)
Pb2—P^iii	4.142 (8)	O1—O2^xvii	3.260 (4)
Pb2—P^iv	4.142 (8)	O1—O2^xviii	3.260 (4)
Pb2—P^xv	3.290 (3)	O1—O2^xix	3.260 (4)
Pb2—P^xvi	3.290 (3)	O1—O2^xx	3.260 (4)
Pb2—P^xvii	3.290 (3)	O1—O2^xxi	3.260 (4)
Pb2—O1	2.381 (8)	O2—Pb1^xiii	2.552 (4)
Pb2—O1^xv	4.048 (5)	O2—Pb2^xv	2.7541 (12)
Pb2—O1^xvi	4.048 (5)	O2—Pb2^xvii	2.7541 (12)
Pb2—O1^xvii	4.048 (5)	O2—Pb2^xiii	2.775 (5)
Pb2—O2^iii	2.775 (5)	O2—P	1.535 (6)
Pb2—O2^viii	2.775 (5)	O2—P^xxii	3.587 (10)
Pb2—O2^ix	2.775 (5)	O2—O1	2.498 (7)
Pb2—O2^xv	2.7541 (12)	O2—O1^xv	3.260 (4)
Pb2—O2^xvii	2.7541 (12)	O2—O1^xvii	3.260 (4)
Pb2—O2^xviii	2.7541 (12)	O2—O2^xxiii	2.506 (8)
Pb2—O2^xix	2.7541 (12)	O2—O2^xxvii	2.887 (8)
Pb2—O2^xx	2.7541 (12)	O2—O2^xxviii	2.887 (8)
Pb2—O2^xxi	2.7541 (12)	O2—O2^xxiv	2.506 (8)
P—Pb1^xii	3.422 (4)	O2—O2^xxii	4.006 (9)
P—Pb1^xiii	3.422 (4)	O2—O2^xxv	3.125 (7)
P—Pb1^xiv	3.422 (4)	O2—O2^xxvi	3.125 (7)
P—Pb2	3.904 (11)
O1—P—O2	109.5 (3)	O2—P—O2^xxiii	109.4 (3)
O1—P—O2^xxiii	109.5 (3)	O2—P—O2^xxiv	109.4 (3)
O1—P—O2^xxiv	109.5 (3)	O2^xxiii—P—O2^xxiv	109.4 (3)

Symmetry codes: (i) −x, −y, −z; (ii) x−2/3, y−1/3, z−1/3; (iii) x+1/3, y−1/3, z−1/3; (iv) x+1/3, y+2/3, z−1/3; (v) −x−2/3, −y−1/3, −z+2/3; (vi) −x−2/3, −y+2/3, −z+2/3; (vii) −x+1/3, −y+2/3, −z+2/3; (viii) −y+1/3, x−y+2/3, z−1/3; (ix) y−x−2/3, −x−1/3, z−1/3; (x) y−2/3, y−x−1/3, −z+2/3; (xi) x−y+1/3, x+2/3, −z+2/3; (xii) x−1/3, y−2/3, z+1/3; (xiii) x−1/3, y+1/3, z+1/3; (xiv) x+2/3, y+1/3, z+1/3; (xv) −x−1/3, −y−2/3, −z+1/3; (xvi) −x+2/3, −y−2/3, −z+1/3; (xvii) −x+2/3, −y+1/3, −z+1/3; (xviii) y−1/3, y−x−2/3, −z+1/3; (xix) y+2/3, y−x−2/3, −z+1/3; (xx) x−y+2/3, x−2/3, −z+1/3; (xxi) x−y+2/3, x+1/3, −z+1/3; (xxii) −x, −y, −z+1; (xxiii) −y, x−y, z; (xxiv) y−x, −x, z; (xxv) y, y−x, −z+1; (xxvi) x−y, x, −z+1; (xxvii) −y, x−y+1, z; (xxviii) y−x−1, −x, z.

(S3P5T_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8952 (9) Å	T = 298 K
c = 2.8294 (13) Å	Particle morphology: Pressure cell anvil material
V = 20.54 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.881 < d < 2.998 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.058	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 64.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.97 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 167.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.043	34 parameters
Rexp = 0.036	0 restraints
R(F^2) = 0.17381	(Δ/σ)max = 0.01
χ^2 = 1.513	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.29615 2: -0.262129 3: 0.585253 4: -9.040860E-02 5: 0.279121 6: -0.111587 7: 0.157996 8: -6.275300E-02 9: 8.944730E-0210: -4.246060E-0211: 3.246880E-0212: -4.863080E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.78149 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.152 (4)	P—Pb2	3.290 (3)
Pb1—Pb2	4.152 (4)	P—Pb2	3.290 (3)
Pb1—Pb2	3.983 (3)	P—Pb2	3.290 (3)
Pb1—Pb2	3.983 (3)	P—Pb2	4.142 (8)
Pb1—Pb2	3.983 (3)	P—Pb2	4.142 (8)
Pb1—Pb2	3.983 (3)	P—Pb2	4.142 (8)
Pb1—Pb2	3.983 (3)	P—P	3.795 (18)
Pb1—Pb2	3.983 (3)	P—O1	1.524 (11)
Pb1—P	3.422 (4)	P—O1	3.381 (4)
Pb1—P	3.422 (4)	P—O1	3.381 (4)
Pb1—P	3.422 (4)	P—O1	3.381 (4)
Pb1—P	3.422 (4)	P—O2	1.535 (6)
Pb1—P	3.422 (4)	P—O2^i	1.535 (6)
Pb1—P	3.422 (4)	P—O2^ii	1.535 (6)
Pb1—O1	3.1151 (3)	P—O2	3.587 (10)
Pb1—O1	3.1151 (3)	P—O2	3.587 (10)
Pb1—O1	3.1151 (3)	P—O2	3.587 (10)
Pb1—O1	3.1151 (3)	O1—Pb1	3.1151 (3)
Pb1—O1	3.1151 (3)	O1—Pb1	3.1151 (3)
Pb1—O1	3.1151 (3)	O1—Pb1	3.1151 (3)
Pb1—O2	2.552 (4)	O1—Pb2	2.381 (8)
Pb1—O2	2.552 (4)	O1—Pb2	4.048 (5)
Pb1—O2	2.552 (4)	O1—Pb2	4.048 (5)
Pb1—O2	2.552 (4)	O1—Pb2	4.048 (5)
Pb1—O2	2.552 (4)	O1—P	1.524 (11)
Pb1—O2	2.552 (4)	O1—P	3.381 (4)
Pb2—Pb1	4.152 (4)	O1—P	3.381 (4)
Pb2—Pb1	3.983 (3)	O1—P	3.381 (4)
Pb2—Pb1	3.983 (3)	O1—O1	3.1202 (9)
Pb2—Pb1	3.983 (3)	O1—O1	3.1202 (9)
Pb2—Pb2	3.532 (4)	O1—O1	3.1202 (9)
Pb2—Pb2	3.532 (4)	O1—O2	2.498 (7)
Pb2—Pb2	3.532 (4)	O1—O2^i	2.498 (7)
Pb2—P	3.904 (11)	O1—O2^ii	2.498 (7)
Pb2—P	4.142 (8)	O1—O2	3.260 (4)
Pb2—P	4.142 (8)	O1—O2	3.260 (4)
Pb2—P	4.142 (8)	O1—O2	3.260 (4)
Pb2—P	3.290 (3)	O1—O2	3.260 (4)
Pb2—P	3.290 (3)	O1—O2	3.260 (4)
Pb2—P	3.290 (3)	O1—O2	3.260 (4)
Pb2—O1	2.381 (8)	O2—Pb1	2.552 (4)
Pb2—O1	4.048 (5)	O2—Pb2	2.7541 (12)
Pb2—O1	4.048 (5)	O2—Pb2	2.7541 (12)
Pb2—O1	4.048 (5)	O2—Pb2	2.775 (5)
Pb2—O2	2.775 (5)	O2—P	1.535 (6)
Pb2—O2	2.775 (5)	O2—P	3.587 (10)
Pb2—O2	2.775 (5)	O2—O1	2.498 (7)
Pb2—O2	2.7541 (12)	O2—O1	3.260 (4)
Pb2—O2	2.7541 (12)	O2—O1	3.260 (4)
Pb2—O2	2.7541 (12)	O2—O2^i	2.506 (8)
Pb2—O2	2.7541 (12)	O2—O2^iii	2.887 (8)
Pb2—O2	2.7541 (12)	O2—O2^iv	2.887 (8)
Pb2—O2	2.7541 (12)	O2—O2^ii	2.506 (8)
P—Pb1	3.422 (4)	O2—O2	4.006 (9)
P—Pb1	3.422 (4)	O2—O2	3.125 (7)
P—Pb1	3.422 (4)	O2—O2	3.125 (7)
P—Pb2	3.904 (11)
O1—P—O2	109.5 (3)	O2—P—O2^i	109.4 (3)
O1—P—O2^i	109.5 (3)	O2—P—O2^ii	109.4 (3)
O1—P—O2^ii	109.5 (3)	O2^i—P—O2^ii	109.4 (3)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) y−x, −x+1, −z; (iv) −y−1, x−y, z.

(S3P5T_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5323 (8) Å	Particle morphology: Component of pressure cell, not sample
V = 44.08 (4) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.881 < d < 2.998 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.058	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 64.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.97 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 167.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.043	34 parameters
Rexp = 0.036	0 restraints
R(F^2) = 0.17381	(Δ/σ)max = 0.01
χ^2 = 1.513	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.29615 2: -0.262129 3: 0.585253 4: -9.040860E-02 5: 0.279121 6: -0.111587 7: 0.157996 8: -6.275300E-02 9: 8.944730E-0210: -4.246060E-0211: 3.246880E-0212: -4.863080E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.78149 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.152 (4)	P—Pb2^xv	3.290 (3)
Pb1—Pb2^i	4.152 (4)	P—Pb2^xvi	3.290 (3)
Pb1—Pb2^ii	3.983 (3)	P—Pb2^xvii	3.290 (3)
Pb1—Pb2^iii	3.983 (3)	P—Pb2^xii	4.142 (8)
Pb1—Pb2^iv	3.983 (3)	P—Pb2^xiii	4.142 (8)
Pb1—Pb2^v	3.983 (3)	P—Pb2^xiv	4.142 (8)
Pb1—Pb2^vi	3.983 (3)	P—P^xxii	3.795 (18)
Pb1—Pb2^vii	3.983 (3)	P—O1	1.524 (11)
Pb1—P^ii	3.422 (4)	P—O1^xv	3.381 (4)
Pb1—P^iii	3.422 (4)	P—O1^xvi	3.381 (4)
Pb1—P^iv	3.422 (4)	P—O1^xvii	3.381 (4)
Pb1—P^v	3.422 (4)	P—O2	1.535 (6)
Pb1—P^vi	3.422 (4)	P—O2^xxiii	1.535 (6)
Pb1—P^vii	3.422 (4)	P—O2^xxiv	1.535 (6)
Pb1—O1^ii	3.1151 (3)	P—O2^xxii	3.587 (10)
Pb1—O1^iii	3.1151 (3)	P—O2^xxv	3.587 (10)
Pb1—O1^iv	3.1151 (3)	P—O2^xxvi	3.587 (10)
Pb1—O1^v	3.1151 (3)	O1—Pb1^xii	3.1151 (3)
Pb1—O1^vi	3.1151 (3)	O1—Pb1^xiii	3.1151 (3)
Pb1—O1^vii	3.1151 (3)	O1—Pb1^xiv	3.1151 (3)
Pb1—O2^iii	2.552 (4)	O1—Pb2	2.381 (8)
Pb1—O2^viii	2.552 (4)	O1—Pb2^xv	4.048 (5)
Pb1—O2^ix	2.552 (4)	O1—Pb2^xvi	4.048 (5)
Pb1—O2^vi	2.552 (4)	O1—Pb2^xvii	4.048 (5)
Pb1—O2^x	2.552 (4)	O1—P	1.524 (11)
Pb1—O2^xi	2.552 (4)	O1—P^xv	3.381 (4)
Pb2—Pb1	4.152 (4)	O1—P^xvi	3.381 (4)
Pb2—Pb1^xii	3.983 (3)	O1—P^xvii	3.381 (4)
Pb2—Pb1^xiii	3.983 (3)	O1—O1^xv	3.1202 (9)
Pb2—Pb1^xiv	3.983 (3)	O1—O1^xvi	3.1202 (9)
Pb2—Pb2^v	3.532 (4)	O1—O1^xvii	3.1202 (9)
Pb2—Pb2^vi	3.532 (4)	O1—O2	2.498 (7)
Pb2—Pb2^vii	3.532 (4)	O1—O2^xxiii	2.498 (7)
Pb2—P	3.904 (11)	O1—O2^xxiv	2.498 (7)
Pb2—P^ii	4.142 (8)	O1—O2^xv	3.260 (4)
Pb2—P^iii	4.142 (8)	O1—O2^xvii	3.260 (4)
Pb2—P^iv	4.142 (8)	O1—O2^xviii	3.260 (4)
Pb2—P^xv	3.290 (3)	O1—O2^xix	3.260 (4)
Pb2—P^xvi	3.290 (3)	O1—O2^xx	3.260 (4)
Pb2—P^xvii	3.290 (3)	O1—O2^xxi	3.260 (4)
Pb2—O1	2.381 (8)	O2—Pb1^xiii	2.552 (4)
Pb2—O1^xv	4.048 (5)	O2—Pb2^xv	2.7541 (12)
Pb2—O1^xvi	4.048 (5)	O2—Pb2^xvii	2.7541 (12)
Pb2—O1^xvii	4.048 (5)	O2—Pb2^xiii	2.775 (5)
Pb2—O2^iii	2.775 (5)	O2—P	1.535 (6)
Pb2—O2^viii	2.775 (5)	O2—P^xxii	3.587 (10)
Pb2—O2^ix	2.775 (5)	O2—O1	2.498 (7)
Pb2—O2^xv	2.7541 (12)	O2—O1^xv	3.260 (4)
Pb2—O2^xvii	2.7541 (12)	O2—O1^xvii	3.260 (4)
Pb2—O2^xviii	2.7541 (12)	O2—O2^xxiii	2.506 (8)
Pb2—O2^xix	2.7541 (12)	O2—O2^xxvii	2.887 (8)
Pb2—O2^xx	2.7541 (12)	O2—O2^xxviii	2.887 (8)
Pb2—O2^xxi	2.7541 (12)	O2—O2^xxiv	2.506 (8)
P—Pb1^xii	3.422 (4)	O2—O2^xxii	4.006 (9)
P—Pb1^xiii	3.422 (4)	O2—O2^xxv	3.125 (7)
P—Pb1^xiv	3.422 (4)	O2—O2^xxvi	3.125 (7)
P—Pb2	3.904 (11)
O1—P—O2	109.5 (3)	O2—P—O2^xxiii	109.4 (3)
O1—P—O2^xxiii	109.5 (3)	O2—P—O2^xxiv	109.4 (3)
O1—P—O2^xxiv	109.5 (3)	O2^xxiii—P—O2^xxiv	109.4 (3)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y−1/2, z−1/2; (iii) x, y−1/2, z−1/2; (iv) x, y+1/2, z−1/2; (v) −x−1/2, −y−1, −z+1/2; (vi) −x−1/2, −y, −z+1/2; (vii) −x+1/2, −y, −z+1/2; (viii) z, x+1/2, y−1/2; (ix) y−1, z−1/2, x−1/2; (x) −z−1/2, −x−1, −y+1/2; (xi) −y+1/2, −z, −x+1/2; (xii) x−1/2, y−1, z+1/2; (xiii) x−1/2, y, z+1/2; (xiv) x+1/2, y, z+1/2; (xv) −x−1, −y−1/2, −z+1/2; (xvi) −x, −y−1/2, −z+1/2; (xvii) −x, −y+1/2, −z+1/2; (xviii) −z−1, −x−1/2, −y+1/2; (xix) −z, −x−1/2, −y+1/2; (xx) −y, −z−1/2, −x+1/2; (xxi) −y, −z+1/2, −x+1/2; (xxii) −x, −y, −z+1; (xxiii) z, x, y; (xxiv) y, z, x; (xxv) −z, −x, −y+1; (xxvi) −y, −z, −x+1; (xxvii) z, x+1, y; (xxviii) y−1, z, x.

(S3P6T_phase_1)

Crystal data

O8P2Pb3	Z = 3
Mr = 811.74	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.3651 (3) Å	Particle morphology: plate
c = 19.8407 (17) Å	irregular, 6 × 6 mm
V = 494.59 (6) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.842 < d < 2.961 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.060	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 61.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 12.25 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.4 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 225.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.046	34 parameters
Rexp = 0.039	0 restraints
R(F^2) = 0.12872	(Δ/σ)max = 0.01
χ^2 = 1.440	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.12873 2: -0.180787 3: 0.454797 4: -3.221780E-02 5: 0.151691 6: -4.867960E-02 7: 5.080020E-02 8: -1.832720E-02 9: 2.429860E-0210: -2.811830E-0211: 1.158700E-0212: -1.085130E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.76430 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.0	0.0	0.0	0.0130 (12)*
Pb2	0.0	0.0	0.2086 (2)	0.0130 (12)*
P	0.0	0.0	0.4042 (5)	0.017 (2)*
O1	0.0	0.0	0.3279 (3)	0.0176 (13)*
O2	−0.1557 (5)	0.1557 (5)	0.4310 (2)	0.0176 (13)*

Geometric parameters (Å, º)

Pb1—Pb2	4.139 (4)	P—Pb2^xvi	3.277 (3)
Pb1—Pb2^i	4.139 (4)	P—Pb2^xvii	3.277 (3)
Pb1—Pb2^ii	3.965 (3)	P—Pb2^xii	4.130 (8)
Pb1—Pb2^iii	3.965 (3)	P—Pb2^xiii	4.130 (8)
Pb1—Pb2^iv	3.965 (3)	P—Pb2^xiv	4.130 (8)
Pb1—Pb2^v	3.965 (3)	P—P^xxii	3.80 (2)
Pb1—Pb2^vi	3.965 (3)	P—P^xv	4.184 (14)
Pb1—Pb2^vii	3.965 (3)	P—P^xvi	4.184 (14)
Pb1—P^ii	3.402 (4)	P—P^xvii	4.184 (14)
Pb1—P^iii	3.402 (4)	P—O1	1.514 (13)
Pb1—P^iv	3.402 (4)	P—O1^xv	3.359 (5)
Pb1—P^v	3.402 (4)	P—O1^xvi	3.359 (5)
Pb1—P^vi	3.402 (4)	P—O1^xvii	3.359 (5)
Pb1—P^vii	3.402 (4)	P—O2	1.541 (6)
Pb1—O1^ii	3.0994 (3)	P—O2^xxiii	1.541 (6)
Pb1—O1^iii	3.0994 (3)	P—O2^xxiv	1.541 (6)
Pb1—O1^iv	3.0994 (3)	P—O2^xxii	3.576 (11)
Pb1—O1^v	3.0994 (3)	P—O2^xxv	3.576 (11)
Pb1—O1^vi	3.0994 (3)	P—O2^xxvi	3.576 (11)
Pb1—O1^vii	3.0994 (3)	O1—Pb1^xii	3.0994 (3)
Pb1—O2^iii	2.545 (5)	O1—Pb1^xiii	3.0994 (3)
Pb1—O2^viii	2.545 (5)	O1—Pb1^xiv	3.0994 (3)
Pb1—O2^ix	2.545 (5)	O1—Pb2	2.367 (8)
Pb1—O2^vi	2.545 (5)	O1—Pb2^xv	4.033 (5)
Pb1—O2^x	2.545 (5)	O1—Pb2^xvi	4.033 (5)
Pb1—O2^xi	2.545 (5)	O1—Pb2^xvii	4.033 (5)
Pb2—Pb1	4.139 (4)	O1—P	1.514 (13)
Pb2—Pb1^xii	3.965 (3)	O1—P^xv	3.359 (5)
Pb2—Pb1^xiii	3.965 (3)	O1—P^xvi	3.359 (5)
Pb2—Pb1^xiv	3.965 (3)	O1—P^xvii	3.359 (5)
Pb2—Pb2^v	3.516 (4)	O1—O1^xv	3.1050 (10)
Pb2—Pb2^vi	3.516 (4)	O1—O1^xvi	3.1050 (10)
Pb2—Pb2^vii	3.516 (4)	O1—O1^xvii	3.1050 (10)
Pb2—P	3.881 (12)	O1—O2	2.505 (8)
Pb2—P^ii	4.130 (8)	O1—O2^xxiii	2.505 (8)
Pb2—P^iii	4.130 (8)	O1—O2^xxiv	2.505 (8)
Pb2—P^iv	4.130 (8)	O1—O2^xv	3.249 (4)
Pb2—P^xv	3.277 (3)	O1—O2^xvii	3.249 (4)
Pb2—P^xvi	3.277 (3)	O1—O2^xviii	3.249 (4)
Pb2—P^xvii	3.277 (3)	O1—O2^xix	3.249 (4)
Pb2—O1	2.367 (8)	O1—O2^xx	3.249 (4)
Pb2—O1^xv	4.033 (5)	O1—O2^xxi	3.249 (4)
Pb2—O1^xvi	4.033 (5)	O2—Pb1^xiii	2.545 (5)
Pb2—O1^xvii	4.033 (5)	O2—Pb2^xv	2.7378 (12)
Pb2—O2^iii	2.752 (5)	O2—Pb2^xvii	2.7378 (12)
Pb2—O2^viii	2.752 (5)	O2—Pb2^xiii	2.752 (5)
Pb2—O2^ix	2.752 (5)	O2—P	1.541 (6)
Pb2—O2^xv	2.7378 (12)	O2—P^xxii	3.576 (11)
Pb2—O2^xvii	2.7378 (12)	O2—O1	2.505 (8)
Pb2—O2^xviii	2.7378 (12)	O2—O1^xv	3.249 (4)
Pb2—O2^xix	2.7378 (12)	O2—O1^xvii	3.249 (4)
Pb2—O2^xx	2.7378 (12)	O2—O2^xxiii	2.506 (9)
Pb2—O2^xxi	2.7378 (12)	O2—O2^xxvii	2.859 (9)
P—Pb1^xii	3.402 (4)	O2—O2^xxviii	2.859 (9)
P—Pb1^xiii	3.402 (4)	O2—O2^xxiv	2.506 (9)
P—Pb1^xiv	3.402 (4)	O2—O2^xxii	3.985 (9)
P—Pb2	3.881 (12)	O2—O2^xxv	3.098 (8)
P—Pb2^xv	3.277 (3)	O2—O2^xxvi	3.098 (8)
O1—P—O2	110.1 (4)	O2—P—O2^xxiii	108.8 (4)
O1—P—O2^xxiii	110.1 (4)	O2—P—O2^xxiv	108.8 (4)
O1—P—O2^xxiv	110.1 (4)	O2^xxiii—P—O2^xxiv	108.8 (4)

Symmetry codes: (i) −x, −y, −z; (ii) x−2/3, y−1/3, z−1/3; (iii) x+1/3, y−1/3, z−1/3; (iv) x+1/3, y+2/3, z−1/3; (v) −x−2/3, −y−1/3, −z+2/3; (vi) −x−2/3, −y+2/3, −z+2/3; (vii) −x+1/3, −y+2/3, −z+2/3; (viii) −y+1/3, x−y+2/3, z−1/3; (ix) y−x−2/3, −x−1/3, z−1/3; (x) y−2/3, y−x−1/3, −z+2/3; (xi) x−y+1/3, x+2/3, −z+2/3; (xii) x−1/3, y−2/3, z+1/3; (xiii) x−1/3, y+1/3, z+1/3; (xiv) x+2/3, y+1/3, z+1/3; (xv) −x−1/3, −y−2/3, −z+1/3; (xvi) −x+2/3, −y−2/3, −z+1/3; (xvii) −x+2/3, −y+1/3, −z+1/3; (xviii) y−1/3, y−x−2/3, −z+1/3; (xix) y+2/3, y−x−2/3, −z+1/3; (xx) x−y+2/3, x−2/3, −z+1/3; (xxi) x−y+2/3, x+1/3, −z+1/3; (xxii) −x, −y, −z+1; (xxiii) −y, x−y, z; (xxiv) y−x, −x, z; (xxv) y, y−x, −z+1; (xxvi) x−y, x, −z+1; (xxvii) −y, x−y+1, z; (xxviii) y−x−1, −x, z.

(S3P6T_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8916 (9) Å	T = 298 K
c = 2.8298 (15) Å	Particle morphology: Pressure cell anvil material
V = 20.49 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.842 < d < 2.961 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.060	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 61.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 12.25 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.4 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 225.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.046	34 parameters
Rexp = 0.039	0 restraints
R(F^2) = 0.12872	(Δ/σ)max = 0.01
χ^2 = 1.440	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.12873 2: -0.180787 3: 0.454797 4: -3.221780E-02 5: 0.151691 6: -4.867960E-02 7: 5.080020E-02 8: -1.832720E-02 9: 2.429860E-0210: -2.811830E-0211: 1.158700E-0212: -1.085130E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.76430 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.139 (4)	P—Pb2	3.277 (3)
Pb1—Pb2	4.139 (4)	P—Pb2	3.277 (3)
Pb1—Pb2	3.965 (3)	P—Pb2	4.130 (8)
Pb1—Pb2	3.965 (3)	P—Pb2	4.130 (8)
Pb1—Pb2	3.965 (3)	P—Pb2	4.130 (8)
Pb1—Pb2	3.965 (3)	P—P	3.80 (2)
Pb1—Pb2	3.965 (3)	P—P	4.184 (14)
Pb1—Pb2	3.965 (3)	P—P	4.184 (14)
Pb1—P	3.402 (4)	P—P	4.184 (14)
Pb1—P	3.402 (4)	P—O1	1.514 (13)
Pb1—P	3.402 (4)	P—O1	3.359 (5)
Pb1—P	3.402 (4)	P—O1	3.359 (5)
Pb1—P	3.402 (4)	P—O1	3.359 (5)
Pb1—P	3.402 (4)	P—O2	1.541 (6)
Pb1—O1	3.0994 (3)	P—O2^i	1.541 (6)
Pb1—O1	3.0994 (3)	P—O2^ii	1.541 (6)
Pb1—O1	3.0994 (3)	P—O2	3.576 (11)
Pb1—O1	3.0994 (3)	P—O2	3.576 (11)
Pb1—O1	3.0994 (3)	P—O2	3.576 (11)
Pb1—O1	3.0994 (3)	O1—Pb1	3.0994 (3)
Pb1—O2	2.545 (5)	O1—Pb1	3.0994 (3)
Pb1—O2	2.545 (5)	O1—Pb1	3.0994 (3)
Pb1—O2	2.545 (5)	O1—Pb2	2.367 (8)
Pb1—O2	2.545 (5)	O1—Pb2	4.033 (5)
Pb1—O2	2.545 (5)	O1—Pb2	4.033 (5)
Pb1—O2	2.545 (5)	O1—Pb2	4.033 (5)
Pb2—Pb1	4.139 (4)	O1—P	1.514 (13)
Pb2—Pb1	3.965 (3)	O1—P	3.359 (5)
Pb2—Pb1	3.965 (3)	O1—P	3.359 (5)
Pb2—Pb1	3.965 (3)	O1—P	3.359 (5)
Pb2—Pb2	3.516 (4)	O1—O1	3.1050 (10)
Pb2—Pb2	3.516 (4)	O1—O1	3.1050 (10)
Pb2—Pb2	3.516 (4)	O1—O1	3.1050 (10)
Pb2—P	3.881 (12)	O1—O2	2.505 (8)
Pb2—P	4.130 (8)	O1—O2^i	2.505 (8)
Pb2—P	4.130 (8)	O1—O2^ii	2.505 (8)
Pb2—P	4.130 (8)	O1—O2	3.249 (4)
Pb2—P	3.277 (3)	O1—O2	3.249 (4)
Pb2—P	3.277 (3)	O1—O2	3.249 (4)
Pb2—P	3.277 (3)	O1—O2	3.249 (4)
Pb2—O1	2.367 (8)	O1—O2	3.249 (4)
Pb2—O1	4.033 (5)	O1—O2	3.249 (4)
Pb2—O1	4.033 (5)	O2—Pb1	2.545 (5)
Pb2—O1	4.033 (5)	O2—Pb2	2.7378 (12)
Pb2—O2	2.752 (5)	O2—Pb2	2.7378 (12)
Pb2—O2	2.752 (5)	O2—Pb2	2.752 (5)
Pb2—O2	2.752 (5)	O2—P	1.541 (6)
Pb2—O2	2.7378 (12)	O2—P	3.576 (11)
Pb2—O2	2.7378 (12)	O2—O1	2.505 (8)
Pb2—O2	2.7378 (12)	O2—O1	3.249 (4)
Pb2—O2	2.7378 (12)	O2—O1	3.249 (4)
Pb2—O2	2.7378 (12)	O2—O2^i	2.506 (9)
Pb2—O2	2.7378 (12)	O2—O2^iii	2.859 (9)
P—Pb1	3.402 (4)	O2—O2^iv	2.859 (9)
P—Pb1	3.402 (4)	O2—O2^ii	2.506 (9)
P—Pb1	3.402 (4)	O2—O2	3.985 (9)
P—Pb2	3.881 (12)	O2—O2	3.098 (8)
P—Pb2	3.277 (3)	O2—O2	3.098 (8)
O1—P—O2	110.1 (4)	O2—P—O2^i	108.8 (4)
O1—P—O2^i	110.1 (4)	O2—P—O2^ii	108.8 (4)
O1—P—O2^ii	110.1 (4)	O2^i—P—O2^ii	108.8 (4)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) y−x, −x+1, −z; (iv) −y−1, x−y, z.

(S3P6T_phase_3)

Crystal data

Ni	material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5276 (9) Å	Particle morphology: Component of pressure cell, not sample
V = 43.90 (4) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), 2.842 < d < 2.961 Angstrom (contamination from unidentified phase), d > 3.734 Angstrom (no useful data)
Rp = 0.060	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 61.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 12.25 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.4 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 225.3 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.50 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.046	34 parameters
Rexp = 0.039	0 restraints
R(F^2) = 0.12872	(Δ/σ)max = 0.01
χ^2 = 1.440	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.12873 2: -0.180787 3: 0.454797 4: -3.221780E-02 5: 0.151691 6: -4.867960E-02 7: 5.080020E-02 8: -1.832720E-02 9: 2.429860E-0210: -2.811830E-0211: 1.158700E-0212: -1.085130E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.76430 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.139 (4)	P—Pb2^xvi	3.277 (3)
Pb1—Pb2^i	4.139 (4)	P—Pb2^xvii	3.277 (3)
Pb1—Pb2^ii	3.965 (3)	P—Pb2^xii	4.130 (8)
Pb1—Pb2^iii	3.965 (3)	P—Pb2^xiii	4.130 (8)
Pb1—Pb2^iv	3.965 (3)	P—Pb2^xiv	4.130 (8)
Pb1—Pb2^v	3.965 (3)	P—P^xxii	3.80 (2)
Pb1—Pb2^vi	3.965 (3)	P—P^xv	4.184 (14)
Pb1—Pb2^vii	3.965 (3)	P—P^xvi	4.184 (14)
Pb1—P^ii	3.402 (4)	P—P^xvii	4.184 (14)
Pb1—P^iii	3.402 (4)	P—O1	1.514 (13)
Pb1—P^iv	3.402 (4)	P—O1^xv	3.359 (5)
Pb1—P^v	3.402 (4)	P—O1^xvi	3.359 (5)
Pb1—P^vi	3.402 (4)	P—O1^xvii	3.359 (5)
Pb1—P^vii	3.402 (4)	P—O2	1.541 (6)
Pb1—O1^ii	3.0994 (3)	P—O2^xxiii	1.541 (6)
Pb1—O1^iii	3.0994 (3)	P—O2^xxiv	1.541 (6)
Pb1—O1^iv	3.0994 (3)	P—O2^xxii	3.576 (11)
Pb1—O1^v	3.0994 (3)	P—O2^xxv	3.576 (11)
Pb1—O1^vi	3.0994 (3)	P—O2^xxvi	3.576 (11)
Pb1—O1^vii	3.0994 (3)	O1—Pb1^xii	3.0994 (3)
Pb1—O2^iii	2.545 (5)	O1—Pb1^xiii	3.0994 (3)
Pb1—O2^viii	2.545 (5)	O1—Pb1^xiv	3.0994 (3)
Pb1—O2^ix	2.545 (5)	O1—Pb2	2.367 (8)
Pb1—O2^vi	2.545 (5)	O1—Pb2^xv	4.033 (5)
Pb1—O2^x	2.545 (5)	O1—Pb2^xvi	4.033 (5)
Pb1—O2^xi	2.545 (5)	O1—Pb2^xvii	4.033 (5)
Pb2—Pb1	4.139 (4)	O1—P	1.514 (13)
Pb2—Pb1^xii	3.965 (3)	O1—P^xv	3.359 (5)
Pb2—Pb1^xiii	3.965 (3)	O1—P^xvi	3.359 (5)
Pb2—Pb1^xiv	3.965 (3)	O1—P^xvii	3.359 (5)
Pb2—Pb2^v	3.516 (4)	O1—O1^xv	3.1050 (10)
Pb2—Pb2^vi	3.516 (4)	O1—O1^xvi	3.1050 (10)
Pb2—Pb2^vii	3.516 (4)	O1—O1^xvii	3.1050 (10)
Pb2—P	3.881 (12)	O1—O2	2.505 (8)
Pb2—P^ii	4.130 (8)	O1—O2^xxiii	2.505 (8)
Pb2—P^iii	4.130 (8)	O1—O2^xxiv	2.505 (8)
Pb2—P^iv	4.130 (8)	O1—O2^xv	3.249 (4)
Pb2—P^xv	3.277 (3)	O1—O2^xvii	3.249 (4)
Pb2—P^xvi	3.277 (3)	O1—O2^xviii	3.249 (4)
Pb2—P^xvii	3.277 (3)	O1—O2^xix	3.249 (4)
Pb2—O1	2.367 (8)	O1—O2^xx	3.249 (4)
Pb2—O1^xv	4.033 (5)	O1—O2^xxi	3.249 (4)
Pb2—O1^xvi	4.033 (5)	O2—Pb1^xiii	2.545 (5)
Pb2—O1^xvii	4.033 (5)	O2—Pb2^xv	2.7378 (12)
Pb2—O2^iii	2.752 (5)	O2—Pb2^xvii	2.7378 (12)
Pb2—O2^viii	2.752 (5)	O2—Pb2^xiii	2.752 (5)
Pb2—O2^ix	2.752 (5)	O2—P	1.541 (6)
Pb2—O2^xv	2.7378 (12)	O2—P^xxii	3.576 (11)
Pb2—O2^xvii	2.7378 (12)	O2—O1	2.505 (8)
Pb2—O2^xviii	2.7378 (12)	O2—O1^xv	3.249 (4)
Pb2—O2^xix	2.7378 (12)	O2—O1^xvii	3.249 (4)
Pb2—O2^xx	2.7378 (12)	O2—O2^xxiii	2.506 (9)
Pb2—O2^xxi	2.7378 (12)	O2—O2^xxvii	2.859 (9)
P—Pb1^xii	3.402 (4)	O2—O2^xxviii	2.859 (9)
P—Pb1^xiii	3.402 (4)	O2—O2^xxiv	2.506 (9)
P—Pb1^xiv	3.402 (4)	O2—O2^xxii	3.985 (9)
P—Pb2	3.881 (12)	O2—O2^xxv	3.098 (8)
P—Pb2^xv	3.277 (3)	O2—O2^xxvi	3.098 (8)
O1—P—O2	110.1 (4)	O2—P—O2^xxiii	108.8 (4)
O1—P—O2^xxiii	110.1 (4)	O2—P—O2^xxiv	108.8 (4)
O1—P—O2^xxiv	110.1 (4)	O2^xxiii—P—O2^xxiv	108.8 (4)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y−1/2, z−1/2; (iii) x, y−1/2, z−1/2; (iv) x, y+1/2, z−1/2; (v) −x−1/2, −y−1, −z+1/2; (vi) −x−1/2, −y, −z+1/2; (vii) −x+1/2, −y, −z+1/2; (viii) z, x+1/2, y−1/2; (ix) y−1, z−1/2, x−1/2; (x) −z−1/2, −x−1, −y+1/2; (xi) −y+1/2, −z, −x+1/2; (xii) x−1/2, y−1, z+1/2; (xiii) x−1/2, y, z+1/2; (xiv) x+1/2, y, z+1/2; (xv) −x−1, −y−1/2, −z+1/2; (xvi) −x, −y−1/2, −z+1/2; (xvii) −x, −y+1/2, −z+1/2; (xviii) −z−1, −x−1/2, −y+1/2; (xix) −z, −x−1/2, −y+1/2; (xx) −y, −z−1/2, −x+1/2; (xxi) −y, −z+1/2, −x+1/2; (xxii) −x, −y, −z+1; (xxiii) z, x, y; (xxiv) y, z, x; (xxv) −z, −x, −y+1; (xxvi) −y, −z, −x+1; (xxvii) z, x+1, y; (xxviii) y−1, z, x.

(S4P7_phase_1)

Crystal data

O8P2Pb3	V = 723.32 (10) Å^3
Mr = 811.54	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.8041 (14) Å	T = 298 K
b = 5.6877 (7) Å	Particle morphology: plate
c = 9.4318 (10) Å	irregular, 6 × 6 mm
β = 102.373 (11)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.047	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 65.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 4.64 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 334.5 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.034	50 parameters
Rexp = 0.028	10 restraints
R(F^2) = 0.21494	(Δ/σ)max < 0.001
χ^2 = 1.488	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.50674 2: -0.309067 3: 0.403204 4: -4.816140E-02 5: 6.532280E-02 6: -2.083650E-02 7: 8.058310E-03 8: -7.322630E-03 9: 1.764640E-0210: -3.351920E-0211: 2.760650E-0212: -1.026830E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.80334 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.0	0.285 (3)	0.25	0.030 (2)*
Pb2	0.3179 (5)	0.3062 (16)	0.3512 (10)	0.030 (2)*
P	0.6035 (4)	0.2591 (15)	0.4495 (7)	0.021 (3)*
O21	0.6510 (8)	0.043 (2)	0.3972 (14)	0.024 (2)*
O22	0.6340 (8)	0.478 (2)	0.3768 (12)	0.024 (2)*
O23	0.6380 (8)	0.282 (2)	0.6141 (10)	0.024 (2)*
O1	0.4917 (6)	0.234 (2)	0.4106 (13)	0.024 (2)*

Geometric parameters (Å, º)

Pb1—Pb2	4.287 (7)	O21—Pb2^x	2.888 (17)
Pb1—Pb2^i	4.287 (7)	O21—Pb2^xi	3.055 (16)
Pb1—Pb2^ii	3.961 (15)	O21—Pb2^xii	4.368 (13)
Pb1—Pb2^iii	4.127 (16)	O21—Pb2^viii	2.781 (13)
Pb1—Pb2^iv	3.961 (15)	O21—Pb2^xiii	4.489 (16)
Pb1—Pb2^v	4.127 (16)	O21—P	1.524 (10)
Pb1—Pb2^vi	4.085 (8)	O21—P^x	4.430 (16)
Pb1—Pb2^vii	4.085 (8)	O21—P^xi	4.424 (15)
Pb1—P^ii	3.659 (15)	O21—P^xviii	4.475 (11)
Pb1—P^iii	3.419 (14)	O21—P^xiv	3.569 (15)
Pb1—P^iv	3.659 (15)	O21—O21^x	4.49 (2)
Pb1—P^v	3.419 (14)	O21—O21^xix	4.48 (2)
Pb1—P^vi	3.446 (6)	O21—O21^xiv	3.81 (2)
Pb1—P^vii	3.446 (6)	O21—O22^xx	3.225 (11)
Pb1—O21^iii	2.680 (14)	O21—O22	2.488 (11)
Pb1—O21^v	2.680 (14)	O21—O22^xxi	4.348 (11)
Pb1—O21^vi	4.398 (11)	O21—O22^xiv	3.264 (17)
Pb1—O21^vii	4.398 (11)	O21—O23	2.493 (11)
Pb1—O22^ii	2.639 (16)	O21—O23^xi	4.377 (15)
Pb1—O22^iii	4.407 (19)	O21—O23^xviii	3.219 (16)
Pb1—O22^iv	2.639 (16)	O21—O23^xiv	3.101 (14)
Pb1—O22^v	4.407 (19)	O21—O1	2.481 (11)
Pb1—O23^vi	2.543 (12)	O21—O1^x	3.322 (14)
Pb1—O23^vii	2.543 (12)	O21—O1^xi	3.345 (16)
Pb1—O1^ii	3.495 (17)	O22—Pb1^viii	4.407 (19)
Pb1—O1^iii	2.982 (18)	O22—Pb1^ix	2.639 (16)
Pb1—O1^iv	3.495 (17)	O22—Pb2	4.428 (12)
Pb1—O1^v	2.982 (18)	O22—Pb2^x	2.575 (15)
Pb1—O1^vi	3.181 (12)	O22—Pb2^xii	2.793 (16)
Pb1—O1^vii	3.181 (12)	O22—Pb2^ix	3.201 (12)
Pb2—Pb1	4.287 (7)	O22—P	1.523 (10)
Pb2—Pb1^viii	4.127 (16)	O22—P^x	4.178 (15)
Pb2—Pb1^ix	3.961 (15)	O22—P^xii	4.240 (15)
Pb2—Pb1^vi	4.085 (8)	O22—P^xvii	4.234 (10)
Pb2—Pb2^iv	3.702 (10)	O22—P^xiv	3.884 (14)
Pb2—Pb2^v	3.702 (10)	O22—O21	2.488 (11)
Pb2—Pb2^vi	3.749 (19)	O22—O21^xxii	3.225 (11)
Pb2—P	3.862 (9)	O22—O21^xxiii	4.348 (11)
Pb2—P^x	3.257 (12)	O22—O21^xiv	3.264 (17)
Pb2—P^xi	3.765 (12)	O22—O22^x	3.95 (2)
Pb2—P^xii	3.154 (12)	O22—O22^xiv	4.38 (2)
Pb2—P^iii	4.174 (12)	O22—O23	2.491 (11)
Pb2—P^vii	4.294 (10)	O22—O23^xii	4.015 (16)
Pb2—O21^x	2.888 (17)	O22—O23^xvii	2.841 (15)
Pb2—O21^xi	3.055 (16)	O22—O23^xiv	3.460 (16)
Pb2—O21^xii	4.368 (13)	O22—O1	2.481 (11)
Pb2—O21^iii	2.781 (13)	O22—O1^x	3.204 (13)
Pb2—O21^vii	4.489 (16)	O22—O1^xii	3.347 (17)
Pb2—O22	4.428 (12)	O23—Pb1^vi	2.543 (12)
Pb2—O22^x	2.575 (15)	O23—Pb2^xi	3.401 (15)
Pb2—O22^xii	2.793 (16)	O23—Pb2^xii	2.427 (15)
Pb2—O22^ii	3.201 (12)	O23—Pb2^xiii	3.005 (11)
Pb2—O23^xi	3.401 (15)	O23—P	1.528 (9)
Pb2—O23^xii	2.427 (15)	O23—P^xi	4.481 (16)
Pb2—O23^vii	3.005 (11)	O23—P^xii	4.177 (16)
Pb2—O1	2.380 (11)	O23—P^xvi	4.208 (14)
Pb2—O1^x	3.995 (14)	O23—P^xiv	3.749 (14)
Pb2—O1^xi	4.345 (14)	O23—O21	2.493 (11)
Pb2—O1^xii	4.033 (15)	O23—O21^xi	4.377 (15)
P—Pb1^viii	3.419 (14)	O23—O21^xv	3.219 (16)
P—Pb1^ix	3.659 (15)	O23—O21^xiv	3.101 (14)
P—Pb1^vi	3.446 (6)	O23—O22	2.491 (11)
P—Pb2	3.862 (9)	O23—O22^xii	4.015 (16)
P—Pb2^x	3.257 (12)	O23—O22^xvi	2.841 (15)
P—Pb2^xi	3.765 (12)	O23—O22^xiv	3.460 (16)
P—Pb2^xii	3.154 (12)	O23—O23^xiv	4.14 (2)
P—Pb2^viii	4.174 (12)	O23—O1	2.485 (9)
P—Pb2^xiii	4.294 (10)	O23—O1^xi	3.418 (18)
P—P^x	4.210 (12)	O23—O1^xii	3.267 (19)
P—P^xi	4.351 (13)	O1—Pb1^viii	2.982 (18)
P—P^xii	4.213 (13)	O1—Pb1^ix	3.495 (17)
P—P^xiv	3.952 (10)	O1—Pb1^vi	3.181 (12)
P—O21	1.524 (10)	O1—Pb2	2.380 (11)
P—O21^x	4.430 (16)	O1—Pb2^x	3.995 (14)
P—O21^xi	4.424 (15)	O1—Pb2^xi	4.345 (14)
P—O21^xv	4.475 (11)	O1—Pb2^xii	4.033 (15)
P—O21^xiv	3.569 (15)	O1—P	1.515 (8)
P—O22	1.523 (10)	O1—P^x	3.372 (15)
P—O22^x	4.178 (15)	O1—P^xi	3.476 (17)
P—O22^xii	4.240 (15)	O1—P^xii	3.538 (17)
P—O22^xvi	4.234 (10)	O1—O21	2.481 (11)
P—O22^xiv	3.884 (14)	O1—O21^x	3.322 (14)
P—O23	1.528 (9)	O1—O21^xi	3.345 (16)
P—O23^xi	4.481 (16)	O1—O22	2.481 (11)
P—O23^xii	4.177 (16)	O1—O22^x	3.204 (13)
P—O23^xvii	4.208 (14)	O1—O22^xii	3.347 (17)
P—O23^xiv	3.749 (14)	O1—O23	2.485 (9)
P—O1	1.515 (8)	O1—O23^xi	3.418 (18)
P—O1^x	3.372 (15)	O1—O23^xii	3.267 (19)
P—O1^xi	3.476 (17)	O1—O1^x	3.09 (2)
P—O1^xii	3.538 (17)	O1—O1^xi	3.13 (2)
O21—Pb1^viii	2.680 (14)	O1—O1^xii	3.45 (3)
O21—Pb1^vi	4.398 (11)
O21—P—O22	109.49 (14)	O22—P—O23	109.44 (13)
O21—P—O23	109.53 (13)	O22—P—O1	109.47 (13)
O21—P—O1	109.42 (14)	O23—P—O1	109.48 (15)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, −y, z+3/2; (xvi) x, −y+1, z+3/2; (xvii) x, −y+1, z+1/2; (xviii) x, −y, z+1/2; (xix) −x+3/2, −y−1/2, −z+1; (xx) x, y−1, z; (xxi) −x+3/2, y−1/2, −z+1/2; (xxii) x, y+1, z; (xxiii) −x+3/2, y+1/2, −z+1/2.

(S4P7_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.9017 (7) Å	T = 298 K
c = 2.8286 (11) Å	Particle morphology: Pressure cell anvil material
V = 20.63 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.047	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 65.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 4.64 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 334.5 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.034	50 parameters
Rexp = 0.028	10 restraints
R(F^2) = 0.21494	(Δ/σ)max < 0.001
χ^2 = 1.488	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.50674 2: -0.309067 3: 0.403204 4: -4.816140E-02 5: 6.532280E-02 6: -2.083650E-02 7: 8.058310E-03 8: -7.322630E-03 9: 1.764640E-0210: -3.351920E-0211: 2.760650E-0212: -1.026830E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.80334 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W(1)	0.0	0.0	0.0	0.025*
C(2)	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.287 (7)	O21—Pb2^ii	2.888 (17)
Pb1—Pb2^i	4.287 (7)	O21—Pb2	3.055 (16)
Pb1—Pb2	3.961 (15)	O21—Pb2	4.368 (13)
Pb1—Pb2	4.127 (16)	O21—Pb2	2.781 (13)
Pb1—Pb2	3.961 (15)	O21—Pb2	4.489 (16)
Pb1—Pb2	4.127 (16)	O21—P	1.524 (10)
Pb1—Pb2	4.085 (8)	O21—P^ii	4.430 (16)
Pb1—Pb2	4.085 (8)	O21—P	4.424 (15)
Pb1—P	3.659 (15)	O21—P	4.475 (11)
Pb1—P	3.419 (14)	O21—P	3.569 (15)
Pb1—P	3.659 (15)	O21—O21^ii	4.49 (2)
Pb1—P	3.419 (14)	O21—O21	4.48 (2)
Pb1—P	3.446 (6)	O21—O21	3.81 (2)
Pb1—P	3.446 (6)	O21—O22^iii	3.225 (11)
Pb1—O21	2.680 (14)	O21—O22	2.488 (11)
Pb1—O21	2.680 (14)	O21—O22	4.348 (11)
Pb1—O21	4.398 (11)	O21—O22	3.264 (17)
Pb1—O21	4.398 (11)	O21—O23	2.493 (11)
Pb1—O22	2.639 (16)	O21—O23	4.377 (15)
Pb1—O22	4.407 (19)	O21—O23	3.219 (16)
Pb1—O22	2.639 (16)	O21—O23	3.101 (14)
Pb1—O22	4.407 (19)	O21—O1	2.481 (11)
Pb1—O23	2.543 (12)	O21—O1^ii	3.322 (14)
Pb1—O23	2.543 (12)	O21—O1	3.345 (16)
Pb1—O1	3.495 (17)	O22—Pb1	4.407 (19)
Pb1—O1	2.982 (18)	O22—Pb1	2.639 (16)
Pb1—O1	3.495 (17)	O22—Pb2	4.428 (12)
Pb1—O1	2.982 (18)	O22—Pb2^ii	2.575 (15)
Pb1—O1	3.181 (12)	O22—Pb2	2.793 (16)
Pb1—O1	3.181 (12)	O22—Pb2	3.201 (12)
Pb2—Pb1	4.287 (7)	O22—P	1.523 (10)
Pb2—Pb1	4.127 (16)	O22—P^ii	4.178 (15)
Pb2—Pb1	3.961 (15)	O22—P	4.240 (15)
Pb2—Pb1	4.085 (8)	O22—P	4.234 (10)
Pb2—Pb2	3.702 (10)	O22—P	3.884 (14)
Pb2—Pb2	3.702 (10)	O22—O21	2.488 (11)
Pb2—Pb2	3.749 (19)	O22—O21^iv	3.225 (11)
Pb2—P	3.862 (9)	O22—O21	4.348 (11)
Pb2—P^ii	3.257 (12)	O22—O21	3.264 (17)
Pb2—P	3.765 (12)	O22—O22^ii	3.95 (2)
Pb2—P	3.154 (12)	O22—O22	4.38 (2)
Pb2—P	4.174 (12)	O22—O23	2.491 (11)
Pb2—P	4.294 (10)	O22—O23	4.015 (16)
Pb2—O21^ii	2.888 (17)	O22—O23	2.841 (15)
Pb2—O21	3.055 (16)	O22—O23	3.460 (16)
Pb2—O21	4.368 (13)	O22—O1	2.481 (11)
Pb2—O21	2.781 (13)	O22—O1^ii	3.204 (13)
Pb2—O21	4.489 (16)	O22—O1	3.347 (17)
Pb2—O22	4.428 (12)	O23—Pb1	2.543 (12)
Pb2—O22^ii	2.575 (15)	O23—Pb2	3.401 (15)
Pb2—O22	2.793 (16)	O23—Pb2	2.427 (15)
Pb2—O22	3.201 (12)	O23—Pb2	3.005 (11)
Pb2—O23	3.401 (15)	O23—P	1.528 (9)
Pb2—O23	2.427 (15)	O23—P	4.481 (16)
Pb2—O23	3.005 (11)	O23—P	4.177 (16)
Pb2—O1	2.380 (11)	O23—P	4.208 (14)
Pb2—O1^ii	3.995 (14)	O23—P	3.749 (14)
Pb2—O1	4.345 (14)	O23—O21	2.493 (11)
Pb2—O1	4.033 (15)	O23—O21	4.377 (15)
P—Pb1	3.419 (14)	O23—O21	3.219 (16)
P—Pb1	3.659 (15)	O23—O21	3.101 (14)
P—Pb1	3.446 (6)	O23—O22	2.491 (11)
P—Pb2	3.862 (9)	O23—O22	4.015 (16)
P—Pb2^ii	3.257 (12)	O23—O22	2.841 (15)
P—Pb2	3.765 (12)	O23—O22	3.460 (16)
P—Pb2	3.154 (12)	O23—O23	4.14 (2)
P—Pb2	4.174 (12)	O23—O1	2.485 (9)
P—Pb2	4.294 (10)	O23—O1	3.418 (18)
P—P^ii	4.210 (12)	O23—O1	3.267 (19)
P—P	4.351 (13)	O1—Pb1	2.982 (18)
P—P	4.213 (13)	O1—Pb1	3.495 (17)
P—P	3.952 (10)	O1—Pb1	3.181 (12)
P—O21	1.524 (10)	O1—Pb2	2.380 (11)
P—O21^ii	4.430 (16)	O1—Pb2^ii	3.995 (14)
P—O21	4.424 (15)	O1—Pb2	4.345 (14)
P—O21	4.475 (11)	O1—Pb2	4.033 (15)
P—O21	3.569 (15)	O1—P	1.515 (8)
P—O22	1.523 (10)	O1—P^ii	3.372 (15)
P—O22^ii	4.178 (15)	O1—P	3.476 (17)
P—O22	4.240 (15)	O1—P	3.538 (17)
P—O22	4.234 (10)	O1—O21	2.481 (11)
P—O22	3.884 (14)	O1—O21^ii	3.322 (14)
P—O23	1.528 (9)	O1—O21	3.345 (16)
P—O23	4.481 (16)	O1—O22	2.481 (11)
P—O23	4.177 (16)	O1—O22^ii	3.204 (13)
P—O23	4.208 (14)	O1—O22	3.347 (17)
P—O23	3.749 (14)	O1—O23	2.485 (9)
P—O1	1.515 (8)	O1—O23	3.418 (18)
P—O1^ii	3.372 (15)	O1—O23	3.267 (19)
P—O1	3.476 (17)	O1—O1^ii	3.09 (2)
P—O1	3.538 (17)	O1—O1	3.13 (2)
O21—Pb1	2.680 (14)	O1—O1	3.45 (3)
O21—Pb1	4.398 (11)
O21—P—O22	109.49 (14)	O22—P—O23	109.44 (13)
O21—P—O23	109.53 (13)	O22—P—O1	109.47 (13)
O21—P—O1	109.42 (14)	O23—P—O1	109.48 (15)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y−1, z; (iv) x, y+1, z.

(S4P7_phase_3)

Crystal data

Ni	anvil material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5513 (10) Å	Particle morphology: Component of pressure cell, not sample
V = 44.79 (4) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.047	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 65.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 4.64 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 199.7 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 334.5 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.034	50 parameters
Rexp = 0.028	10 restraints
R(F^2) = 0.21494	(Δ/σ)max < 0.001
χ^2 = 1.488	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.50674 2: -0.309067 3: 0.403204 4: -4.816140E-02 5: 6.532280E-02 6: -2.083650E-02 7: 8.058310E-03 8: -7.322630E-03 9: 1.764640E-0210: -3.351920E-0211: 2.760650E-0212: -1.026830E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.80334 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.287 (7)	O21—Pb2^x	2.888 (17)
Pb1—Pb2^i	4.287 (7)	O21—Pb2^xi	3.055 (16)
Pb1—Pb2^ii	3.961 (15)	O21—Pb2^xii	4.368 (13)
Pb1—Pb2^iii	4.127 (16)	O21—Pb2^viii	2.781 (13)
Pb1—Pb2^iv	3.961 (15)	O21—Pb2^xiii	4.489 (16)
Pb1—Pb2^v	4.127 (16)	O21—P	1.524 (10)
Pb1—Pb2^vi	4.085 (8)	O21—P^x	4.430 (16)
Pb1—Pb2^vii	4.085 (8)	O21—P^xi	4.424 (15)
Pb1—P^ii	3.659 (15)	O21—P^xviii	4.475 (11)
Pb1—P^iii	3.419 (14)	O21—P^xiv	3.569 (15)
Pb1—P^iv	3.659 (15)	O21—O21^x	4.49 (2)
Pb1—P^v	3.419 (14)	O21—O21^xix	4.48 (2)
Pb1—P^vi	3.446 (6)	O21—O21^xiv	3.81 (2)
Pb1—P^vii	3.446 (6)	O21—O22^xx	3.225 (11)
Pb1—O21^iii	2.680 (14)	O21—O22	2.488 (11)
Pb1—O21^v	2.680 (14)	O21—O22^xxi	4.348 (11)
Pb1—O21^vi	4.398 (11)	O21—O22^xiv	3.264 (17)
Pb1—O21^vii	4.398 (11)	O21—O23	2.493 (11)
Pb1—O22^ii	2.639 (16)	O21—O23^xi	4.377 (15)
Pb1—O22^iii	4.407 (19)	O21—O23^xviii	3.219 (16)
Pb1—O22^iv	2.639 (16)	O21—O23^xiv	3.101 (14)
Pb1—O22^v	4.407 (19)	O21—O1	2.481 (11)
Pb1—O23^vi	2.543 (12)	O21—O1^x	3.322 (14)
Pb1—O23^vii	2.543 (12)	O21—O1^xi	3.345 (16)
Pb1—O1^ii	3.495 (17)	O22—Pb1^viii	4.407 (19)
Pb1—O1^iii	2.982 (18)	O22—Pb1^ix	2.639 (16)
Pb1—O1^iv	3.495 (17)	O22—Pb2	4.428 (12)
Pb1—O1^v	2.982 (18)	O22—Pb2^x	2.575 (15)
Pb1—O1^vi	3.181 (12)	O22—Pb2^xii	2.793 (16)
Pb1—O1^vii	3.181 (12)	O22—Pb2^ix	3.201 (12)
Pb2—Pb1	4.287 (7)	O22—P	1.523 (10)
Pb2—Pb1^viii	4.127 (16)	O22—P^x	4.178 (15)
Pb2—Pb1^ix	3.961 (15)	O22—P^xii	4.240 (15)
Pb2—Pb1^vi	4.085 (8)	O22—P^xvii	4.234 (10)
Pb2—Pb2^iv	3.702 (10)	O22—P^xiv	3.884 (14)
Pb2—Pb2^v	3.702 (10)	O22—O21	2.488 (11)
Pb2—Pb2^vi	3.749 (19)	O22—O21^xxii	3.225 (11)
Pb2—P	3.862 (9)	O22—O21^xxiii	4.348 (11)
Pb2—P^x	3.257 (12)	O22—O21^xiv	3.264 (17)
Pb2—P^xi	3.765 (12)	O22—O22^x	3.95 (2)
Pb2—P^xii	3.154 (12)	O22—O22^xiv	4.38 (2)
Pb2—P^iii	4.174 (12)	O22—O23	2.491 (11)
Pb2—P^vii	4.294 (10)	O22—O23^xii	4.015 (16)
Pb2—O21^x	2.888 (17)	O22—O23^xvii	2.841 (15)
Pb2—O21^xi	3.055 (16)	O22—O23^xiv	3.460 (16)
Pb2—O21^xii	4.368 (13)	O22—O1	2.481 (11)
Pb2—O21^iii	2.781 (13)	O22—O1^x	3.204 (13)
Pb2—O21^vii	4.489 (16)	O22—O1^xii	3.347 (17)
Pb2—O22	4.428 (12)	O23—Pb1^vi	2.543 (12)
Pb2—O22^x	2.575 (15)	O23—Pb2^xi	3.401 (15)
Pb2—O22^xii	2.793 (16)	O23—Pb2^xii	2.427 (15)
Pb2—O22^ii	3.201 (12)	O23—Pb2^xiii	3.005 (11)
Pb2—O23^xi	3.401 (15)	O23—P	1.528 (9)
Pb2—O23^xii	2.427 (15)	O23—P^xi	4.481 (16)
Pb2—O23^vii	3.005 (11)	O23—P^xii	4.177 (16)
Pb2—O1	2.380 (11)	O23—P^xvi	4.208 (14)
Pb2—O1^x	3.995 (14)	O23—P^xiv	3.749 (14)
Pb2—O1^xi	4.345 (14)	O23—O21	2.493 (11)
Pb2—O1^xii	4.033 (15)	O23—O21^xi	4.377 (15)
P—Pb1^viii	3.419 (14)	O23—O21^xv	3.219 (16)
P—Pb1^ix	3.659 (15)	O23—O21^xiv	3.101 (14)
P—Pb1^vi	3.446 (6)	O23—O22	2.491 (11)
P—Pb2	3.862 (9)	O23—O22^xii	4.015 (16)
P—Pb2^x	3.257 (12)	O23—O22^xvi	2.841 (15)
P—Pb2^xi	3.765 (12)	O23—O22^xiv	3.460 (16)
P—Pb2^xii	3.154 (12)	O23—O23^xiv	4.14 (2)
P—Pb2^viii	4.174 (12)	O23—O1	2.485 (9)
P—Pb2^xiii	4.294 (10)	O23—O1^xi	3.418 (18)
P—P^x	4.210 (12)	O23—O1^xii	3.267 (19)
P—P^xi	4.351 (13)	O1—Pb1^viii	2.982 (18)
P—P^xii	4.213 (13)	O1—Pb1^ix	3.495 (17)
P—P^xiv	3.952 (10)	O1—Pb1^vi	3.181 (12)
P—O21	1.524 (10)	O1—Pb2	2.380 (11)
P—O21^x	4.430 (16)	O1—Pb2^x	3.995 (14)
P—O21^xi	4.424 (15)	O1—Pb2^xi	4.345 (14)
P—O21^xv	4.475 (11)	O1—Pb2^xii	4.033 (15)
P—O21^xiv	3.569 (15)	O1—P	1.515 (8)
P—O22	1.523 (10)	O1—P^x	3.372 (15)
P—O22^x	4.178 (15)	O1—P^xi	3.476 (17)
P—O22^xii	4.240 (15)	O1—P^xii	3.538 (17)
P—O22^xvi	4.234 (10)	O1—O21	2.481 (11)
P—O22^xiv	3.884 (14)	O1—O21^x	3.322 (14)
P—O23	1.528 (9)	O1—O21^xi	3.345 (16)
P—O23^xi	4.481 (16)	O1—O22	2.481 (11)
P—O23^xii	4.177 (16)	O1—O22^x	3.204 (13)
P—O23^xvii	4.208 (14)	O1—O22^xii	3.347 (17)
P—O23^xiv	3.749 (14)	O1—O23	2.485 (9)
P—O1	1.515 (8)	O1—O23^xi	3.418 (18)
P—O1^x	3.372 (15)	O1—O23^xii	3.267 (19)
P—O1^xi	3.476 (17)	O1—O1^x	3.09 (2)
P—O1^xii	3.538 (17)	O1—O1^xi	3.13 (2)
O21—Pb1^viii	2.680 (14)	O1—O1^xii	3.45 (3)
O21—Pb1^vi	4.398 (11)
O21—P—O22	109.49 (14)	O22—P—O23	109.44 (13)
O21—P—O23	109.53 (13)	O22—P—O1	109.47 (13)
O21—P—O1	109.42 (14)	O23—P—O1	109.48 (15)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) −z, −x, −y+1; (xvi) −z, −x+1, −y+1; (xvii) −z, −x+1, −y; (xviii) −z, −x, −y; (xix) −x+1, −y−1/2, −z+3/2; (xx) x, y−1, z; (xxi) z+1, x−1/2, y+1/2; (xxii) x, y+1, z; (xxiii) z+1, x+1/2, y+1/2.

(S4P12_phase_1)

Crystal data

O8P2Pb3	V = 710.71 (10) Å^3
Mr = 811.54	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7881 (15) Å	T = 298 K
b = 5.5967 (7) Å	Particle morphology: plate
c = 9.4441 (9) Å	irregular, 6 × 6 mm
β = 102.788 (13)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 58.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.69 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 136.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 459.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	50 parameters
Rexp = 0.029	10 restraints
R(F^2) = 0.21329	(Δ/σ)max = 0.01
χ^2 = 1.513	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.79307 2: -0.551784 3: 0.633811 4: -0.211483 5: 0.211561 6: -0.134454 7: 0.106617 8: -8.836690E-02 9: 8.383180E-0210: -8.362710E-0211: 5.561150E-0212: -2.146230E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.82962 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.0	0.278 (3)	0.25	0.030 (2)*
Pb2	0.3155 (5)	0.2973 (19)	0.3518 (12)	0.030 (2)*
P	0.6037 (3)	0.2581 (18)	0.4512 (7)	0.017 (3)*
O21	0.6481 (9)	0.029 (2)	0.3980 (15)	0.0199 (18)*
O22	0.6392 (10)	0.478 (3)	0.3799 (14)	0.0199 (18)*
O23	0.6380 (9)	0.278 (3)	0.6161 (11)	0.0199 (18)*
O1	0.4916 (5)	0.245 (3)	0.4101 (14)	0.0199 (18)*

Geometric parameters (Å, º)

Pb1—Pb2	4.244 (6)	O21—Pb1^vi	4.404 (13)
Pb1—Pb2^i	4.244 (6)	O21—Pb2^x	2.931 (19)
Pb1—Pb2^ii	3.963 (18)	O21—Pb2^xi	2.942 (18)
Pb1—Pb2^iii	4.115 (18)	O21—Pb2^xii	4.418 (14)
Pb1—Pb2^iv	3.963 (18)	O21—Pb2^viii	2.766 (14)
Pb1—Pb2^v	4.115 (18)	O21—P^xvii	4.404 (11)
Pb1—Pb2^vi	4.069 (10)	O21—P	1.550 (10)
Pb1—Pb2^vii	4.069 (10)	O21—P^x	4.416 (16)
Pb1—P^ii	3.592 (16)	O21—P^xi	4.343 (17)
Pb1—P^iii	3.419 (16)	O21—P^xix	4.430 (11)
Pb1—P^iv	3.592 (16)	O21—P^xiv	3.605 (16)
Pb1—P^v	3.419 (16)	O21—O21^x	4.41 (3)
Pb1—P^vi	3.440 (7)	O21—O21^xxi	4.36 (3)
Pb1—P^vii	3.440 (7)	O21—O21^xiv	3.91 (3)
Pb1—O21^iii	2.616 (17)	O21—O22^xvii	3.089 (11)
Pb1—O21^v	2.616 (17)	O21—O22	2.520 (11)
Pb1—O21^vi	4.404 (13)	O21—O22^xxii	4.356 (12)
Pb1—O21^vii	4.404 (13)	O21—O22^xiv	3.206 (17)
Pb1—O22^ii	2.636 (18)	O21—O23	2.514 (11)
Pb1—O22^iii	4.42 (2)	O21—O23^xi	4.277 (18)
Pb1—O22^iv	2.636 (18)	O21—O23^xix	3.146 (17)
Pb1—O22^v	4.42 (2)	O21—O23^xiv	3.172 (18)
Pb1—O23^vi	2.526 (13)	O21—O1	2.498 (11)
Pb1—O23^vii	2.526 (13)	O21—O1^x	3.340 (14)
Pb1—O1^ii	3.35 (2)	O21—O1^xi	3.302 (18)
Pb1—O1^iii	3.04 (2)	O22—Pb1^viii	4.42 (2)
Pb1—O1^iv	3.35 (2)	O22—Pb1^ix	2.636 (18)
Pb1—O1^v	3.04 (2)	O22—Pb2^x	2.609 (19)
Pb1—O1^vi	3.189 (13)	O22—Pb2^xii	2.773 (19)
Pb1—O1^vii	3.189 (13)	O22—Pb2^ix	3.074 (12)
Pb2—Pb1	4.244 (6)	O22—P	1.536 (10)
Pb2—Pb1^viii	4.115 (18)	O22—P^xv	4.459 (12)
Pb2—Pb1^ix	3.963 (18)	O22—P^x	4.228 (16)
Pb2—Pb1^vi	4.069 (10)	O22—P^xii	4.278 (19)
Pb2—Pb2^iv	3.640 (11)	O22—P^xx	4.234 (11)
Pb2—Pb2^v	3.640 (11)	O22—P^xiv	3.789 (17)
Pb2—Pb2^vi	3.69 (2)	O22—O21	2.520 (11)
Pb2—P	3.882 (8)	O22—O21^xv	3.089 (11)
Pb2—P^x	3.299 (14)	O22—O21^xxiii	4.356 (12)
Pb2—P^xi	3.667 (13)	O22—O21^xiv	3.206 (17)
Pb2—P^xii	3.159 (14)	O22—O22^x	4.07 (3)
Pb2—P^ii	4.442 (12)	O22—O22^xiv	4.24 (3)
Pb2—P^iii	4.156 (12)	O22—O23	2.501 (11)
Pb2—P^vii	4.248 (11)	O22—O23^xii	4.067 (18)
Pb2—O21^x	2.931 (19)	O22—O23^xx	2.838 (16)
Pb2—O21^xi	2.942 (18)	O22—O23^xiv	3.382 (18)
Pb2—O21^xii	4.418 (14)	O22—O1	2.486 (11)
Pb2—O21^iii	2.766 (14)	O22—O1^x	3.205 (14)
Pb2—O22^x	2.609 (19)	O22—O1^xii	3.34 (2)
Pb2—O22^xii	2.773 (19)	O23—Pb1^vi	2.526 (13)
Pb2—O22^ii	3.074 (12)	O23—Pb2^xi	3.281 (15)
Pb2—O23^xi	3.281 (15)	O23—Pb2^xii	2.466 (15)
Pb2—O23^xii	2.466 (15)	O23—Pb2^xiii	2.951 (11)
Pb2—O23^vii	2.951 (11)	O23—P	1.528 (9)
Pb2—O1	2.385 (10)	O23—P^xi	4.423 (18)
Pb2—O1^x	4.024 (16)	O23—P^xii	4.162 (17)
Pb2—O1^xi	4.325 (17)	O23—P^xvi	4.460 (17)
Pb2—O1^xii	4.004 (17)	O23—P^xviii	4.202 (15)
P—Pb1^viii	3.419 (16)	O23—P^xiv	3.759 (14)
P—Pb1^ix	3.592 (16)	O23—O21	2.514 (11)
P—Pb1^vi	3.440 (7)	O23—O21^xi	4.277 (18)
P—Pb2	3.882 (8)	O23—O21^xvi	3.146 (17)
P—Pb2^x	3.299 (14)	O23—O21^xiv	3.172 (18)
P—Pb2^xi	3.667 (13)	O23—O22	2.501 (11)
P—Pb2^xii	3.159 (14)	O23—O22^xii	4.067 (18)
P—Pb2^viii	4.156 (12)	O23—O22^xviii	2.838 (16)
P—Pb2^ix	4.442 (12)	O23—O22^xiv	3.382 (18)
P—Pb2^xiii	4.248 (11)	O23—O23^xiv	4.18 (2)
P—P^x	4.220 (12)	O23—O1	2.480 (9)
P—P^xi	4.306 (15)	O23—O1^xi	3.41 (2)
P—P^xii	4.187 (16)	O23—O1^xii	3.19 (2)
P—P^xiv	3.935 (9)	O1—Pb1^viii	3.04 (2)
P—O21	1.550 (10)	O1—Pb1^ix	3.35 (2)
P—O21^xv	4.404 (11)	O1—Pb1^vi	3.189 (13)
P—O21^x	4.416 (16)	O1—Pb2	2.385 (10)
P—O21^xi	4.343 (17)	O1—Pb2^x	4.024 (16)
P—O21^xvi	4.430 (11)	O1—Pb2^xi	4.325 (17)
P—O21^xiv	3.605 (16)	O1—Pb2^xii	4.004 (17)
P—O22^xvii	4.459 (12)	O1—P	1.510 (8)
P—O22	1.536 (10)	O1—P^x	3.375 (16)
P—O22^x	4.228 (16)	O1—P^xi	3.49 (2)
P—O22^xii	4.278 (19)	O1—P^xii	3.45 (2)
P—O22^xviii	4.234 (11)	O1—O21	2.498 (11)
P—O22^xiv	3.789 (17)	O1—O21^x	3.340 (14)
P—O23	1.528 (9)	O1—O21^xi	3.302 (18)
P—O23^xi	4.423 (18)	O1—O22	2.486 (11)
P—O23^xii	4.162 (17)	O1—O22^x	3.205 (14)
P—O23^xix	4.460 (17)	O1—O22^xii	3.34 (2)
P—O23^xx	4.202 (15)	O1—O23	2.480 (9)
P—O23^xiv	3.759 (14)	O1—O23^xi	3.41 (2)
P—O1	1.510 (8)	O1—O23^xii	3.19 (2)
P—O1^x	3.375 (16)	O1—O1^x	3.08 (3)
P—O1^xi	3.49 (2)	O1—O1^xi	3.21 (3)
P—O1^xii	3.45 (2)	O1—O1^xii	3.30 (3)
O21—Pb1^viii	2.616 (17)
O21—P—O22	109.52 (14)	O22—P—O23	109.46 (14)
O21—P—O23	109.51 (14)	O22—P—O1	109.45 (14)
O21—P—O1	109.44 (15)	O23—P—O1	109.44 (15)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, y−1, z; (xviii) x, −y+1, z+3/2; (xix) x, −y, z+1/2; (xx) x, −y+1, z+1/2; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2.

(S4P12_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.9003 (7) Å	T = 298 K
c = 2.8311 Å	Particle morphology: Pressure cell anvil material
V = 20.63 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 58.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.69 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 136.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 459.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	50 parameters
Rexp = 0.029	10 restraints
R(F^2) = 0.21329	(Δ/σ)max = 0.01
χ^2 = 1.513	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.79307 2: -0.551784 3: 0.633811 4: -0.211483 5: 0.211561 6: -0.134454 7: 0.106617 8: -8.836690E-02 9: 8.383180E-0210: -8.362710E-0211: 5.561150E-0212: -2.146230E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.82962 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W(1)	0.0	0.0	0.0	0.025*
C(2)	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.244 (6)	O21—Pb1	4.404 (13)
Pb1—Pb2^i	4.244 (6)	O21—Pb2^ii	2.931 (19)
Pb1—Pb2	3.963 (18)	O21—Pb2	2.942 (18)
Pb1—Pb2	4.115 (18)	O21—Pb2	4.418 (14)
Pb1—Pb2	3.963 (18)	O21—Pb2	2.766 (14)
Pb1—Pb2	4.115 (18)	O21—P^iv	4.404 (11)
Pb1—Pb2	4.069 (10)	O21—P	1.550 (10)
Pb1—Pb2	4.069 (10)	O21—P^ii	4.416 (16)
Pb1—P	3.592 (16)	O21—P	4.343 (17)
Pb1—P	3.419 (16)	O21—P	4.430 (11)
Pb1—P	3.592 (16)	O21—P	3.605 (16)
Pb1—P	3.419 (16)	O21—O21^ii	4.41 (3)
Pb1—P	3.440 (7)	O21—O21	4.36 (3)
Pb1—P	3.440 (7)	O21—O21	3.91 (3)
Pb1—O21	2.616 (17)	O21—O22^iv	3.089 (11)
Pb1—O21	2.616 (17)	O21—O22	2.520 (11)
Pb1—O21	4.404 (13)	O21—O22	4.356 (12)
Pb1—O21	4.404 (13)	O21—O22	3.206 (17)
Pb1—O22	2.636 (18)	O21—O23	2.514 (11)
Pb1—O22	4.42 (2)	O21—O23	4.277 (18)
Pb1—O22	2.636 (18)	O21—O23	3.146 (17)
Pb1—O22	4.42 (2)	O21—O23	3.172 (18)
Pb1—O23	2.526 (13)	O21—O1	2.498 (11)
Pb1—O23	2.526 (13)	O21—O1^ii	3.340 (14)
Pb1—O1	3.35 (2)	O21—O1	3.302 (18)
Pb1—O1	3.04 (2)	O22—Pb1	4.42 (2)
Pb1—O1	3.35 (2)	O22—Pb1	2.636 (18)
Pb1—O1	3.04 (2)	O22—Pb2^ii	2.609 (19)
Pb1—O1	3.189 (13)	O22—Pb2	2.773 (19)
Pb1—O1	3.189 (13)	O22—Pb2	3.074 (12)
Pb2—Pb1	4.244 (6)	O22—P	1.536 (10)
Pb2—Pb1	4.115 (18)	O22—P^iii	4.459 (12)
Pb2—Pb1	3.963 (18)	O22—P^ii	4.228 (16)
Pb2—Pb1	4.069 (10)	O22—P	4.278 (19)
Pb2—Pb2	3.640 (11)	O22—P	4.234 (11)
Pb2—Pb2	3.640 (11)	O22—P	3.789 (17)
Pb2—Pb2	3.69 (2)	O22—O21	2.520 (11)
Pb2—P	3.882 (8)	O22—O21^iii	3.089 (11)
Pb2—P^ii	3.299 (14)	O22—O21	4.356 (12)
Pb2—P	3.667 (13)	O22—O21	3.206 (17)
Pb2—P	3.159 (14)	O22—O22^ii	4.07 (3)
Pb2—P	4.442 (12)	O22—O22	4.24 (3)
Pb2—P	4.156 (12)	O22—O23	2.501 (11)
Pb2—P	4.248 (11)	O22—O23	4.067 (18)
Pb2—O21^ii	2.931 (19)	O22—O23	2.838 (16)
Pb2—O21	2.942 (18)	O22—O23	3.382 (18)
Pb2—O21	4.418 (14)	O22—O1	2.486 (11)
Pb2—O21	2.766 (14)	O22—O1^ii	3.205 (14)
Pb2—O22^ii	2.609 (19)	O22—O1	3.34 (2)
Pb2—O22	2.773 (19)	O23—Pb1	2.526 (13)
Pb2—O22	3.074 (12)	O23—Pb2	3.281 (15)
Pb2—O23	3.281 (15)	O23—Pb2	2.466 (15)
Pb2—O23	2.466 (15)	O23—Pb2	2.951 (11)
Pb2—O23	2.951 (11)	O23—P	1.528 (9)
Pb2—O1	2.385 (10)	O23—P	4.423 (18)
Pb2—O1^ii	4.024 (16)	O23—P	4.162 (17)
Pb2—O1	4.325 (17)	O23—P	4.460 (17)
Pb2—O1	4.004 (17)	O23—P	4.202 (15)
P—Pb1	3.419 (16)	O23—P	3.759 (14)
P—Pb1	3.592 (16)	O23—O21	2.514 (11)
P—Pb1	3.440 (7)	O23—O21	4.277 (18)
P—Pb2	3.882 (8)	O23—O21	3.146 (17)
P—Pb2^ii	3.299 (14)	O23—O21	3.172 (18)
P—Pb2	3.667 (13)	O23—O22	2.501 (11)
P—Pb2	3.159 (14)	O23—O22	4.067 (18)
P—Pb2	4.156 (12)	O23—O22	2.838 (16)
P—Pb2	4.442 (12)	O23—O22	3.382 (18)
P—Pb2	4.248 (11)	O23—O23	4.18 (2)
P—P^ii	4.220 (12)	O23—O1	2.480 (9)
P—P	4.306 (15)	O23—O1	3.41 (2)
P—P	4.187 (16)	O23—O1	3.19 (2)
P—P	3.935 (9)	O1—Pb1	3.04 (2)
P—O21	1.550 (10)	O1—Pb1	3.35 (2)
P—O21^iii	4.404 (11)	O1—Pb1	3.189 (13)
P—O21^ii	4.416 (16)	O1—Pb2	2.385 (10)
P—O21	4.343 (17)	O1—Pb2^ii	4.024 (16)
P—O21	4.430 (11)	O1—Pb2	4.325 (17)
P—O21	3.605 (16)	O1—Pb2	4.004 (17)
P—O22^iv	4.459 (12)	O1—P	1.510 (8)
P—O22	1.536 (10)	O1—P^ii	3.375 (16)
P—O22^ii	4.228 (16)	O1—P	3.49 (2)
P—O22	4.278 (19)	O1—P	3.45 (2)
P—O22	4.234 (11)	O1—O21	2.498 (11)
P—O22	3.789 (17)	O1—O21^ii	3.340 (14)
P—O23	1.528 (9)	O1—O21	3.302 (18)
P—O23	4.423 (18)	O1—O22	2.486 (11)
P—O23	4.162 (17)	O1—O22^ii	3.205 (14)
P—O23	4.460 (17)	O1—O22	3.34 (2)
P—O23	4.202 (15)	O1—O23	2.480 (9)
P—O23	3.759 (14)	O1—O23	3.41 (2)
P—O1	1.510 (8)	O1—O23	3.19 (2)
P—O1^ii	3.375 (16)	O1—O1^ii	3.08 (3)
P—O1	3.49 (2)	O1—O1	3.21 (3)
P—O1	3.45 (2)	O1—O1	3.30 (3)
O21—Pb1	2.616 (17)
O21—P—O22	109.52 (14)	O22—P—O23	109.46 (14)
O21—P—O23	109.51 (14)	O22—P—O1	109.45 (14)
O21—P—O1	109.44 (15)	O23—P—O1	109.44 (15)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(S4P12_phase_3)

Crystal data

Ni	anvil material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5507 (10) Å	Particle morphology: Component of pressure cell, not sample
V = 44.77 (4) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 58.8 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.69 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 136.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 459.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	50 parameters
Rexp = 0.029	10 restraints
R(F^2) = 0.21329	(Δ/σ)max = 0.01
χ^2 = 1.513	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.79307 2: -0.551784 3: 0.633811 4: -0.211483 5: 0.211561 6: -0.134454 7: 0.106617 8: -8.836690E-02 9: 8.383180E-0210: -8.362710E-0211: 5.561150E-0212: -2.146230E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.82962 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.244 (6)	O21—Pb1^vi	4.404 (13)
Pb1—Pb2^i	4.244 (6)	O21—Pb2^x	2.931 (19)
Pb1—Pb2^ii	3.963 (18)	O21—Pb2^xi	2.942 (18)
Pb1—Pb2^iii	4.115 (18)	O21—Pb2^xii	4.418 (14)
Pb1—Pb2^iv	3.963 (18)	O21—Pb2^viii	2.766 (14)
Pb1—Pb2^v	4.115 (18)	O21—P^xvii	4.404 (11)
Pb1—Pb2^vi	4.069 (10)	O21—P	1.550 (10)
Pb1—Pb2^vii	4.069 (10)	O21—P^x	4.416 (16)
Pb1—P^ii	3.592 (16)	O21—P^xi	4.343 (17)
Pb1—P^iii	3.419 (16)	O21—P^xix	4.430 (11)
Pb1—P^iv	3.592 (16)	O21—P^xiv	3.605 (16)
Pb1—P^v	3.419 (16)	O21—O21^x	4.41 (3)
Pb1—P^vi	3.440 (7)	O21—O21^xxi	4.36 (3)
Pb1—P^vii	3.440 (7)	O21—O21^xiv	3.91 (3)
Pb1—O21^iii	2.616 (17)	O21—O22^xvii	3.089 (11)
Pb1—O21^v	2.616 (17)	O21—O22	2.520 (11)
Pb1—O21^vi	4.404 (13)	O21—O22^xxii	4.356 (12)
Pb1—O21^vii	4.404 (13)	O21—O22^xiv	3.206 (17)
Pb1—O22^ii	2.636 (18)	O21—O23	2.514 (11)
Pb1—O22^iii	4.42 (2)	O21—O23^xi	4.277 (18)
Pb1—O22^iv	2.636 (18)	O21—O23^xix	3.146 (17)
Pb1—O22^v	4.42 (2)	O21—O23^xiv	3.172 (18)
Pb1—O23^vi	2.526 (13)	O21—O1	2.498 (11)
Pb1—O23^vii	2.526 (13)	O21—O1^x	3.340 (14)
Pb1—O1^ii	3.35 (2)	O21—O1^xi	3.302 (18)
Pb1—O1^iii	3.04 (2)	O22—Pb1^viii	4.42 (2)
Pb1—O1^iv	3.35 (2)	O22—Pb1^ix	2.636 (18)
Pb1—O1^v	3.04 (2)	O22—Pb2^x	2.609 (19)
Pb1—O1^vi	3.189 (13)	O22—Pb2^xii	2.773 (19)
Pb1—O1^vii	3.189 (13)	O22—Pb2^ix	3.074 (12)
Pb2—Pb1	4.244 (6)	O22—P	1.536 (10)
Pb2—Pb1^viii	4.115 (18)	O22—P^xv	4.459 (12)
Pb2—Pb1^ix	3.963 (18)	O22—P^x	4.228 (16)
Pb2—Pb1^vi	4.069 (10)	O22—P^xii	4.278 (19)
Pb2—Pb2^iv	3.640 (11)	O22—P^xx	4.234 (11)
Pb2—Pb2^v	3.640 (11)	O22—P^xiv	3.789 (17)
Pb2—Pb2^vi	3.69 (2)	O22—O21	2.520 (11)
Pb2—P	3.882 (8)	O22—O21^xv	3.089 (11)
Pb2—P^x	3.299 (14)	O22—O21^xxiii	4.356 (12)
Pb2—P^xi	3.667 (13)	O22—O21^xiv	3.206 (17)
Pb2—P^xii	3.159 (14)	O22—O22^x	4.07 (3)
Pb2—P^ii	4.442 (12)	O22—O22^xiv	4.24 (3)
Pb2—P^iii	4.156 (12)	O22—O23	2.501 (11)
Pb2—P^vii	4.248 (11)	O22—O23^xii	4.067 (18)
Pb2—O21^x	2.931 (19)	O22—O23^xx	2.838 (16)
Pb2—O21^xi	2.942 (18)	O22—O23^xiv	3.382 (18)
Pb2—O21^xii	4.418 (14)	O22—O1	2.486 (11)
Pb2—O21^iii	2.766 (14)	O22—O1^x	3.205 (14)
Pb2—O22^x	2.609 (19)	O22—O1^xii	3.34 (2)
Pb2—O22^xii	2.773 (19)	O23—Pb1^vi	2.526 (13)
Pb2—O22^ii	3.074 (12)	O23—Pb2^xi	3.281 (15)
Pb2—O23^xi	3.281 (15)	O23—Pb2^xii	2.466 (15)
Pb2—O23^xii	2.466 (15)	O23—Pb2^xiii	2.951 (11)
Pb2—O23^vii	2.951 (11)	O23—P	1.528 (9)
Pb2—O1	2.385 (10)	O23—P^xi	4.423 (18)
Pb2—O1^x	4.024 (16)	O23—P^xii	4.162 (17)
Pb2—O1^xi	4.325 (17)	O23—P^xvi	4.460 (17)
Pb2—O1^xii	4.004 (17)	O23—P^xviii	4.202 (15)
P—Pb1^viii	3.419 (16)	O23—P^xiv	3.759 (14)
P—Pb1^ix	3.592 (16)	O23—O21	2.514 (11)
P—Pb1^vi	3.440 (7)	O23—O21^xi	4.277 (18)
P—Pb2	3.882 (8)	O23—O21^xvi	3.146 (17)
P—Pb2^x	3.299 (14)	O23—O21^xiv	3.172 (18)
P—Pb2^xi	3.667 (13)	O23—O22	2.501 (11)
P—Pb2^xii	3.159 (14)	O23—O22^xii	4.067 (18)
P—Pb2^viii	4.156 (12)	O23—O22^xviii	2.838 (16)
P—Pb2^ix	4.442 (12)	O23—O22^xiv	3.382 (18)
P—Pb2^xiii	4.248 (11)	O23—O23^xiv	4.18 (2)
P—P^x	4.220 (12)	O23—O1	2.480 (9)
P—P^xi	4.306 (15)	O23—O1^xi	3.41 (2)
P—P^xii	4.187 (16)	O23—O1^xii	3.19 (2)
P—P^xiv	3.935 (9)	O1—Pb1^viii	3.04 (2)
P—O21	1.550 (10)	O1—Pb1^ix	3.35 (2)
P—O21^xv	4.404 (11)	O1—Pb1^vi	3.189 (13)
P—O21^x	4.416 (16)	O1—Pb2	2.385 (10)
P—O21^xi	4.343 (17)	O1—Pb2^x	4.024 (16)
P—O21^xvi	4.430 (11)	O1—Pb2^xi	4.325 (17)
P—O21^xiv	3.605 (16)	O1—Pb2^xii	4.004 (17)
P—O22^xvii	4.459 (12)	O1—P	1.510 (8)
P—O22	1.536 (10)	O1—P^x	3.375 (16)
P—O22^x	4.228 (16)	O1—P^xi	3.49 (2)
P—O22^xii	4.278 (19)	O1—P^xii	3.45 (2)
P—O22^xviii	4.234 (11)	O1—O21	2.498 (11)
P—O22^xiv	3.789 (17)	O1—O21^x	3.340 (14)
P—O23	1.528 (9)	O1—O21^xi	3.302 (18)
P—O23^xi	4.423 (18)	O1—O22	2.486 (11)
P—O23^xii	4.162 (17)	O1—O22^x	3.205 (14)
P—O23^xix	4.460 (17)	O1—O22^xii	3.34 (2)
P—O23^xx	4.202 (15)	O1—O23	2.480 (9)
P—O23^xiv	3.759 (14)	O1—O23^xi	3.41 (2)
P—O1	1.510 (8)	O1—O23^xii	3.19 (2)
P—O1^x	3.375 (16)	O1—O1^x	3.08 (3)
P—O1^xi	3.49 (2)	O1—O1^xi	3.21 (3)
P—O1^xii	3.45 (2)	O1—O1^xii	3.30 (3)
O21—Pb1^viii	2.616 (17)
O21—P—O22	109.52 (14)	O22—P—O23	109.46 (14)
O21—P—O23	109.51 (14)	O22—P—O1	109.45 (14)
O21—P—O1	109.44 (15)	O23—P—O1	109.44 (15)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) x, y+1, z; (xvi) −z, −x, −y+1; (xvii) x, y−1, z; (xviii) −z, −x+1, −y+1; (xix) −z, −x, −y; (xx) −z, −x+1, −y; (xxi) −x+1, −y−1/2, −z+3/2; (xxii) z+1, x−1/2, y+1/2; (xxiii) z+1, x+1/2, y+1/2.

(S4P19MONO_phase_1)

Crystal data

O8P2Pb3	V = 697.83 (10) Å^3
Mr = 811.54	Z = 4
Monoclinic, C2/c	none
Hall symbol: -C 2yc	? radiation
a = 13.7645 (14) Å	T = 298 K
b = 5.5059 (7) Å	Particle morphology: plate
c = 9.4551 (10) Å	irregular, 6 × 6 mm
β = 103.126 (15)°

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 58.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.68 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 119.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 276.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	48 parameters
Rexp = 0.029	10 restraints
R(F^2) = 0.21591	(Δ/σ)max = 0.27
χ^2 = 1.562	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.60700 2: -0.367019 3: 0.462668 4: -6.537410E-02 5: 0.119791 6: -5.489280E-02 7: 6.454060E-02 8: -3.858930E-02 9: 5.409830E-0210: -4.314010E-0211: 2.807320E-0212: -3.586500E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.79989 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pb1	0.0	0.262 (4)	0.25	0.029 (2)*
Pb2	0.3160 (3)	0.287 (2)	0.357 (2)	0.029 (2)*
P	0.6055 (3)	0.260 (2)	0.4520 (10)	0.0057 (17)*
O21	0.6476 (12)	0.026 (3)	0.3988 (18)	0.0185 (15)*
O22	0.6446 (12)	0.480 (3)	0.3846 (17)	0.0185 (15)*
O23	0.6382 (10)	0.275 (3)	0.6168 (13)	0.0185 (15)*
O1	0.4929 (5)	0.255 (3)	0.4073 (19)	0.0185 (15)*

Geometric parameters (Å, º)

Pb1—Pb2	4.237 (5)	O21—Pb2^x	2.95 (3)
Pb1—Pb2^i	4.237 (5)	O21—Pb2^xi	2.84 (2)
Pb1—Pb2^ii	3.93 (2)	O21—Pb2^xii	4.405 (18)
Pb1—Pb2^iii	4.12 (2)	O21—Pb2^viii	2.772 (16)
Pb1—Pb2^iv	3.93 (2)	O21—P^xvii	4.303 (13)
Pb1—Pb2^v	4.12 (2)	O21—P	1.543 (10)
Pb1—Pb2^vi	4.006 (15)	O21—P^x	4.421 (19)
Pb1—Pb2^vii	4.006 (15)	O21—P^xi	4.34 (2)
Pb1—P^ii	3.484 (18)	O21—P^xix	4.421 (13)
Pb1—P^iii	3.465 (19)	O21—P^xiv	3.57 (2)
Pb1—P^iv	3.484 (18)	O21—O21^x	4.39 (3)
Pb1—P^v	3.465 (19)	O21—O21^xxi	4.29 (3)
Pb1—P^vi	3.452 (9)	O21—O21^xiv	3.90 (3)
Pb1—P^vii	3.452 (9)	O21—O22^xvii	3.006 (11)
Pb1—O21^iii	2.63 (2)	O21—O22	2.506 (11)
Pb1—O21^v	2.63 (2)	O21—O22^xxii	4.347 (15)
Pb1—O21^vi	4.425 (16)	O21—O22^xiv	3.12 (2)
Pb1—O21^vii	4.425 (16)	O21—O23	2.504 (10)
Pb1—O22^ii	2.61 (2)	O21—O23^xi	4.24 (2)
Pb1—O22^iii	4.48 (2)	O21—O23^xix	3.12 (2)
Pb1—O22^iv	2.61 (2)	O21—O23^xiv	3.18 (2)
Pb1—O22^v	4.48 (2)	O21—O1	2.493 (11)
Pb1—O23^ii	4.454 (19)	O21—O1^x	3.342 (17)
Pb1—O23^iv	4.454 (19)	O21—O1^xi	3.33 (2)
Pb1—O23^vi	2.517 (15)	O22—Pb1^viii	4.48 (2)
Pb1—O23^vii	2.517 (15)	O22—Pb1^ix	2.61 (2)
Pb1—O1^ii	3.17 (2)	O22—Pb2^x	2.68 (3)
Pb1—O1^iii	3.11 (3)	O22—Pb2^xii	2.71 (3)
Pb1—O1^iv	3.17 (2)	O22—Pb2^ix	2.959 (15)
Pb1—O1^v	3.11 (3)	O22—P	1.526 (10)
Pb1—O1^vi	3.221 (18)	O22—P^xv	4.389 (14)
Pb1—O1^vii	3.221 (18)	O22—P^x	4.30 (2)
Pb2—Pb1	4.237 (5)	O22—P^xii	4.32 (2)
Pb2—Pb1^viii	4.12 (2)	O22—P^xx	4.250 (12)
Pb2—Pb1^ix	3.93 (2)	O22—P^xiv	3.68 (2)
Pb2—Pb1^vi	4.006 (15)	O22—O21	2.506 (11)
Pb2—Pb2^iv	3.643 (17)	O22—O21^xv	3.006 (11)
Pb2—Pb2^v	3.643 (17)	O22—O21^xxiii	4.347 (15)
Pb2—Pb2^vi	3.61 (3)	O22—O21^xiv	3.12 (2)
Pb2—P	3.884 (6)	O22—O22^x	4.21 (3)
Pb2—P^x	3.34 (2)	O22—O22^xiv	4.09 (4)
Pb2—P^xi	3.551 (16)	O22—O22^xxiv	4.37 (3)
Pb2—P^xii	3.130 (17)	O22—O23	2.489 (11)
Pb2—P^ii	4.337 (15)	O22—O23^xii	4.12 (2)
Pb2—P^iii	4.146 (13)	O22—O23^xx	2.851 (17)
Pb2—P^vii	4.249 (15)	O22—O23^xiv	3.31 (2)
Pb2—O21^x	2.95 (3)	O22—O1	2.480 (11)
Pb2—O21^xi	2.84 (2)	O22—O1^x	3.219 (19)
Pb2—O21^xii	4.405 (18)	O22—O1^xii	3.36 (3)
Pb2—O21^iii	2.772 (16)	O23—Pb1^ix	4.454 (19)
Pb2—O22^x	2.68 (3)	O23—Pb1^vi	2.517 (15)
Pb2—O22^xii	2.71 (3)	O23—Pb2^xi	3.154 (16)
Pb2—O22^ii	2.959 (15)	O23—Pb2^xii	2.493 (16)
Pb2—O23^xi	3.154 (16)	O23—Pb2^xiii	2.952 (14)
Pb2—O23^xii	2.493 (16)	O23—P	1.523 (10)
Pb2—O23^vii	2.952 (14)	O23—P^xi	4.400 (19)
Pb2—O1	2.379 (8)	O23—P^xii	4.153 (19)
Pb2—O1^x	4.02 (2)	O23—P^xvi	4.423 (18)
Pb2—O1^xi	4.26 (2)	O23—P^xviii	4.178 (16)
Pb2—O1^xii	3.95 (2)	O23—P^xiv	3.735 (17)
P—Pb1^viii	3.465 (19)	O23—O21	2.504 (10)
P—Pb1^ix	3.484 (18)	O23—O21^xi	4.24 (2)
P—Pb1^vi	3.452 (9)	O23—O21^xvi	3.12 (2)
P—Pb2	3.884 (6)	O23—O21^xiv	3.18 (2)
P—Pb2^x	3.34 (2)	O23—O22	2.489 (11)
P—Pb2^xi	3.551 (16)	O23—O22^xii	4.12 (2)
P—Pb2^xii	3.130 (17)	O23—O22^xviii	2.851 (17)
P—Pb2^viii	4.146 (13)	O23—O22^xiv	3.31 (2)
P—Pb2^ix	4.337 (15)	O23—O23^xxv	4.457 (19)
P—Pb2^xiii	4.249 (15)	O23—O23^xxvi	4.457 (19)
P—P^x	4.241 (16)	O23—O23^xiv	4.19 (3)
P—P^xi	4.317 (17)	O23—O1	2.478 (10)
P—P^xii	4.177 (17)	O23—O1^xi	3.41 (2)
P—P^xiv	3.876 (8)	O23—O1^xii	3.13 (2)
P—O21	1.543 (10)	O1—Pb1^viii	3.11 (3)
P—O21^xv	4.303 (13)	O1—Pb1^ix	3.17 (2)
P—O21^x	4.421 (19)	O1—Pb1^vi	3.221 (18)
P—O21^xi	4.34 (2)	O1—Pb2	2.379 (8)
P—O21^xvi	4.421 (13)	O1—Pb2^x	4.02 (2)
P—O21^xiv	3.57 (2)	O1—Pb2^xi	4.26 (2)
P—O22^xvii	4.389 (14)	O1—Pb2^xii	3.95 (2)
P—O22	1.526 (10)	O1—P	1.511 (7)
P—O22^x	4.30 (2)	O1—P^x	3.36 (2)
P—O22^xii	4.32 (2)	O1—P^xi	3.53 (2)
P—O22^xviii	4.250 (12)	O1—P^xii	3.40 (2)
P—O22^xiv	3.68 (2)	O1—O21	2.493 (11)
P—O23	1.523 (10)	O1—O21^x	3.342 (17)
P—O23^xi	4.400 (19)	O1—O21^xi	3.33 (2)
P—O23^xii	4.153 (19)	O1—O22	2.480 (11)
P—O23^xix	4.423 (18)	O1—O22^x	3.219 (19)
P—O23^xx	4.178 (16)	O1—O22^xii	3.36 (3)
P—O23^xiv	3.735 (17)	O1—O23	2.478 (10)
P—O1	1.511 (7)	O1—O23^xi	3.41 (2)
P—O1^x	3.36 (2)	O1—O23^xii	3.13 (2)
P—O1^xi	3.53 (2)	O1—O1^x	3.03 (4)
P—O1^xii	3.40 (2)	O1—O1^xi	3.30 (4)
O21—Pb1^viii	2.63 (2)	O1—O1^xii	3.20 (4)
O21—Pb1^vi	4.425 (16)
O21—P—O22	109.50 (16)	O22—P—O23	109.46 (15)
O21—P—O23	109.47 (15)	O22—P—O1	109.48 (15)
O21—P—O1	109.45 (16)	O23—P—O1	109.47 (16)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) x+1/2, y+1/2, z; (x) −x+1, y, −z+1/2; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) x+1/2, −y+1/2, z+3/2; (xiv) −x+3/2, −y+1/2, −z+1; (xv) x, y+1, z; (xvi) x, −y, z+3/2; (xvii) x, y−1, z; (xviii) x, −y+1, z+3/2; (xix) x, −y, z+1/2; (xx) x, −y+1, z+1/2; (xxi) −x+3/2, −y−1/2, −z+1; (xxii) −x+3/2, y−1/2, −z+1/2; (xxiii) −x+3/2, y+1/2, −z+1/2; (xxiv) −x+3/2, −y+3/2, −z+1; (xxv) −x+3/2, y−1/2, −z+3/2; (xxvi) −x+3/2, y+1/2, −z+3/2.

(S4P19MONO_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.9008 (6) Å	T = 298 K
c = 2.8295 (10) Å	Particle morphology: Pressure cell anvil material
V = 20.62 (5) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 58.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.68 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 119.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 276.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	48 parameters
Rexp = 0.029	10 restraints
R(F^2) = 0.21591	(Δ/σ)max = 0.27
χ^2 = 1.562	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.60700 2: -0.367019 3: 0.462668 4: -6.537410E-02 5: 0.119791 6: -5.489280E-02 7: 6.454060E-02 8: -3.858930E-02 9: 5.409830E-0210: -4.314010E-0211: 2.807320E-0212: -3.586500E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.79989 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W(1)	0.0	0.0	0.0	0.025*
C(2)	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.237 (5)	O21—Pb2^ii	2.95 (3)
Pb1—Pb2^i	4.237 (5)	O21—Pb2	2.84 (2)
Pb1—Pb2	3.93 (2)	O21—Pb2	4.405 (18)
Pb1—Pb2	4.12 (2)	O21—Pb2	2.772 (16)
Pb1—Pb2	3.93 (2)	O21—P^iv	4.303 (13)
Pb1—Pb2	4.12 (2)	O21—P	1.543 (10)
Pb1—Pb2	4.006 (15)	O21—P^ii	4.421 (19)
Pb1—Pb2	4.006 (15)	O21—P	4.34 (2)
Pb1—P	3.484 (18)	O21—P	4.421 (13)
Pb1—P	3.465 (19)	O21—P	3.57 (2)
Pb1—P	3.484 (18)	O21—O21^ii	4.39 (3)
Pb1—P	3.465 (19)	O21—O21	4.29 (3)
Pb1—P	3.452 (9)	O21—O21	3.90 (3)
Pb1—P	3.452 (9)	O21—O22^iv	3.006 (11)
Pb1—O21	2.63 (2)	O21—O22	2.506 (11)
Pb1—O21	2.63 (2)	O21—O22	4.347 (15)
Pb1—O21	4.425 (16)	O21—O22	3.12 (2)
Pb1—O21	4.425 (16)	O21—O23	2.504 (10)
Pb1—O22	2.61 (2)	O21—O23	4.24 (2)
Pb1—O22	4.48 (2)	O21—O23	3.12 (2)
Pb1—O22	2.61 (2)	O21—O23	3.18 (2)
Pb1—O22	4.48 (2)	O21—O1	2.493 (11)
Pb1—O23	4.454 (19)	O21—O1^ii	3.342 (17)
Pb1—O23	4.454 (19)	O21—O1	3.33 (2)
Pb1—O23	2.517 (15)	O22—Pb1	4.48 (2)
Pb1—O23	2.517 (15)	O22—Pb1	2.61 (2)
Pb1—O1	3.17 (2)	O22—Pb2^ii	2.68 (3)
Pb1—O1	3.11 (3)	O22—Pb2	2.71 (3)
Pb1—O1	3.17 (2)	O22—Pb2	2.959 (15)
Pb1—O1	3.11 (3)	O22—P	1.526 (10)
Pb1—O1	3.221 (18)	O22—P^iii	4.389 (14)
Pb1—O1	3.221 (18)	O22—P^ii	4.30 (2)
Pb2—Pb1	4.237 (5)	O22—P	4.32 (2)
Pb2—Pb1	4.12 (2)	O22—P	4.250 (12)
Pb2—Pb1	3.93 (2)	O22—P	3.68 (2)
Pb2—Pb1	4.006 (15)	O22—O21	2.506 (11)
Pb2—Pb2	3.643 (17)	O22—O21^iii	3.006 (11)
Pb2—Pb2	3.643 (17)	O22—O21	4.347 (15)
Pb2—Pb2	3.61 (3)	O22—O21	3.12 (2)
Pb2—P	3.884 (6)	O22—O22^ii	4.21 (3)
Pb2—P^ii	3.34 (2)	O22—O22	4.09 (4)
Pb2—P	3.551 (16)	O22—O22	4.37 (3)
Pb2—P	3.130 (17)	O22—O23	2.489 (11)
Pb2—P	4.337 (15)	O22—O23	4.12 (2)
Pb2—P	4.146 (13)	O22—O23	2.851 (17)
Pb2—P	4.249 (15)	O22—O23	3.31 (2)
Pb2—O21^ii	2.95 (3)	O22—O1	2.480 (11)
Pb2—O21	2.84 (2)	O22—O1^ii	3.219 (19)
Pb2—O21	4.405 (18)	O22—O1	3.36 (3)
Pb2—O21	2.772 (16)	O23—Pb1	4.454 (19)
Pb2—O22^ii	2.68 (3)	O23—Pb1	2.517 (15)
Pb2—O22	2.71 (3)	O23—Pb2	3.154 (16)
Pb2—O22	2.959 (15)	O23—Pb2	2.493 (16)
Pb2—O23	3.154 (16)	O23—Pb2	2.952 (14)
Pb2—O23	2.493 (16)	O23—P	1.523 (10)
Pb2—O23	2.952 (14)	O23—P	4.400 (19)
Pb2—O1	2.379 (8)	O23—P	4.153 (19)
Pb2—O1^ii	4.02 (2)	O23—P	4.423 (18)
Pb2—O1	4.26 (2)	O23—P	4.178 (16)
Pb2—O1	3.95 (2)	O23—P	3.735 (17)
P—Pb1	3.465 (19)	O23—O21	2.504 (10)
P—Pb1	3.484 (18)	O23—O21	4.24 (2)
P—Pb1	3.452 (9)	O23—O21	3.12 (2)
P—Pb2	3.884 (6)	O23—O21	3.18 (2)
P—Pb2^ii	3.34 (2)	O23—O22	2.489 (11)
P—Pb2	3.551 (16)	O23—O22	4.12 (2)
P—Pb2	3.130 (17)	O23—O22	2.851 (17)
P—Pb2	4.146 (13)	O23—O22	3.31 (2)
P—Pb2	4.337 (15)	O23—O23	4.457 (19)
P—Pb2	4.249 (15)	O23—O23	4.457 (19)
P—P^ii	4.241 (16)	O23—O23	4.19 (3)
P—P	4.317 (17)	O23—O1	2.478 (10)
P—P	4.177 (17)	O23—O1	3.41 (2)
P—P	3.876 (8)	O23—O1	3.13 (2)
P—O21	1.543 (10)	O1—Pb1	3.11 (3)
P—O21^iii	4.303 (13)	O1—Pb1	3.17 (2)
P—O21^ii	4.421 (19)	O1—Pb1	3.221 (18)
P—O21	4.34 (2)	O1—Pb2	2.379 (8)
P—O21	4.421 (13)	O1—Pb2^ii	4.02 (2)
P—O21	3.57 (2)	O1—Pb2	4.26 (2)
P—O22^iv	4.389 (14)	O1—Pb2	3.95 (2)
P—O22	1.526 (10)	O1—P	1.511 (7)
P—O22^ii	4.30 (2)	O1—P^ii	3.36 (2)
P—O22	4.32 (2)	O1—P	3.53 (2)
P—O22	4.250 (12)	O1—P	3.40 (2)
P—O22	3.68 (2)	O1—O21	2.493 (11)
P—O23	1.523 (10)	O1—O21^ii	3.342 (17)
P—O23	4.400 (19)	O1—O21	3.33 (2)
P—O23	4.153 (19)	O1—O22	2.480 (11)
P—O23	4.423 (18)	O1—O22^ii	3.219 (19)
P—O23	4.178 (16)	O1—O22	3.36 (3)
P—O23	3.735 (17)	O1—O23	2.478 (10)
P—O1	1.511 (7)	O1—O23	3.41 (2)
P—O1^ii	3.36 (2)	O1—O23	3.13 (2)
P—O1	3.53 (2)	O1—O1^ii	3.03 (4)
P—O1	3.40 (2)	O1—O1	3.30 (4)
O21—Pb1	2.63 (2)	O1—O1	3.20 (4)
O21—Pb1	4.425 (16)
O21—P—O22	109.50 (16)	O22—P—O23	109.46 (15)
O21—P—O23	109.47 (15)	O22—P—O1	109.48 (15)
O21—P—O1	109.45 (16)	O23—P—O1	109.47 (16)

Symmetry codes: (i) y−x, −x, −z; (ii) y−x+1, −x, −z; (iii) x, y+1, z; (iv) x, y−1, z.

(S4P19MONO_phase_3)

Crystal data

Ni	V = 44.64 (4) Å^3
Mr = 58.71	Z = 4
Cubic, Fm3m	? radiation
a = 3.5474 (9) Å	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.046	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 58.9 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 6.68 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 119.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 276.0 #6 (sig-2) = 8.0 #7 (gam-0) = 0.00 #8 (gam-1) = 5.49 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	48 parameters
Rexp = 0.029	10 restraints
R(F^2) = 0.21591	(Δ/σ)max = 0.27
χ^2 = 1.562	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.60700 2: -0.367019 3: 0.462668 4: -6.537410E-02 5: 0.119791 6: -5.489280E-02 7: 6.454060E-02 8: -3.858930E-02 9: 5.409830E-0210: -4.314010E-0211: 2.807320E-0212: -3.586500E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.79989 h= 1.000 k= 0.000 l= 0.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

Pb1—Pb2	4.237 (5)	O21—Pb2^x	2.95 (3)
Pb1—Pb2^i	4.237 (5)	O21—Pb2^xi	2.84 (2)
Pb1—Pb2^ii	3.93 (2)	O21—Pb2^xii	4.405 (18)
Pb1—Pb2^iii	4.12 (2)	O21—Pb2^viii	2.772 (16)
Pb1—Pb2^iv	3.93 (2)	O21—P^xvii	4.303 (13)
Pb1—Pb2^v	4.12 (2)	O21—P	1.543 (10)
Pb1—Pb2^vi	4.006 (15)	O21—P^x	4.421 (19)
Pb1—Pb2^vii	4.006 (15)	O21—P^xi	4.34 (2)
Pb1—P^ii	3.484 (18)	O21—P^xix	4.421 (13)
Pb1—P^iii	3.465 (19)	O21—P^xiv	3.57 (2)
Pb1—P^iv	3.484 (18)	O21—O21^x	4.39 (3)
Pb1—P^v	3.465 (19)	O21—O21^xxi	4.29 (3)
Pb1—P^vi	3.452 (9)	O21—O21^xiv	3.90 (3)
Pb1—P^vii	3.452 (9)	O21—O22^xvii	3.006 (11)
Pb1—O21^iii	2.63 (2)	O21—O22	2.506 (11)
Pb1—O21^v	2.63 (2)	O21—O22^xxii	4.347 (15)
Pb1—O21^vi	4.425 (16)	O21—O22^xiv	3.12 (2)
Pb1—O21^vii	4.425 (16)	O21—O23	2.504 (10)
Pb1—O22^ii	2.61 (2)	O21—O23^xi	4.24 (2)
Pb1—O22^iii	4.48 (2)	O21—O23^xix	3.12 (2)
Pb1—O22^iv	2.61 (2)	O21—O23^xiv	3.18 (2)
Pb1—O22^v	4.48 (2)	O21—O1	2.493 (11)
Pb1—O23^ii	4.454 (19)	O21—O1^x	3.342 (17)
Pb1—O23^iv	4.454 (19)	O21—O1^xi	3.33 (2)
Pb1—O23^vi	2.517 (15)	O22—Pb1^viii	4.48 (2)
Pb1—O23^vii	2.517 (15)	O22—Pb1^ix	2.61 (2)
Pb1—O1^ii	3.17 (2)	O22—Pb2^x	2.68 (3)
Pb1—O1^iii	3.11 (3)	O22—Pb2^xii	2.71 (3)
Pb1—O1^iv	3.17 (2)	O22—Pb2^ix	2.959 (15)
Pb1—O1^v	3.11 (3)	O22—P	1.526 (10)
Pb1—O1^vi	3.221 (18)	O22—P^xv	4.389 (14)
Pb1—O1^vii	3.221 (18)	O22—P^x	4.30 (2)
Pb2—Pb1	4.237 (5)	O22—P^xii	4.32 (2)
Pb2—Pb1^viii	4.12 (2)	O22—P^xx	4.250 (12)
Pb2—Pb1^ix	3.93 (2)	O22—P^xiv	3.68 (2)
Pb2—Pb1^vi	4.006 (15)	O22—O21	2.506 (11)
Pb2—Pb2^iv	3.643 (17)	O22—O21^xv	3.006 (11)
Pb2—Pb2^v	3.643 (17)	O22—O21^xxiii	4.347 (15)
Pb2—Pb2^vi	3.61 (3)	O22—O21^xiv	3.12 (2)
Pb2—P	3.884 (6)	O22—O22^x	4.21 (3)
Pb2—P^x	3.34 (2)	O22—O22^xiv	4.09 (4)
Pb2—P^xi	3.551 (16)	O22—O22^xxiv	4.37 (3)
Pb2—P^xii	3.130 (17)	O22—O23	2.489 (11)
Pb2—P^ii	4.337 (15)	O22—O23^xii	4.12 (2)
Pb2—P^iii	4.146 (13)	O22—O23^xx	2.851 (17)
Pb2—P^vii	4.249 (15)	O22—O23^xiv	3.31 (2)
Pb2—O21^x	2.95 (3)	O22—O1	2.480 (11)
Pb2—O21^xi	2.84 (2)	O22—O1^x	3.219 (19)
Pb2—O21^xii	4.405 (18)	O22—O1^xii	3.36 (3)
Pb2—O21^iii	2.772 (16)	O23—Pb1^ix	4.454 (19)
Pb2—O22^x	2.68 (3)	O23—Pb1^vi	2.517 (15)
Pb2—O22^xii	2.71 (3)	O23—Pb2^xi	3.154 (16)
Pb2—O22^ii	2.959 (15)	O23—Pb2^xii	2.493 (16)
Pb2—O23^xi	3.154 (16)	O23—Pb2^xiii	2.952 (14)
Pb2—O23^xii	2.493 (16)	O23—P	1.523 (10)
Pb2—O23^vii	2.952 (14)	O23—P^xi	4.400 (19)
Pb2—O1	2.379 (8)	O23—P^xii	4.153 (19)
Pb2—O1^x	4.02 (2)	O23—P^xvi	4.423 (18)
Pb2—O1^xi	4.26 (2)	O23—P^xviii	4.178 (16)
Pb2—O1^xii	3.95 (2)	O23—P^xiv	3.735 (17)
P—Pb1^viii	3.465 (19)	O23—O21	2.504 (10)
P—Pb1^ix	3.484 (18)	O23—O21^xi	4.24 (2)
P—Pb1^vi	3.452 (9)	O23—O21^xvi	3.12 (2)
P—Pb2	3.884 (6)	O23—O21^xiv	3.18 (2)
P—Pb2^x	3.34 (2)	O23—O22	2.489 (11)
P—Pb2^xi	3.551 (16)	O23—O22^xii	4.12 (2)
P—Pb2^xii	3.130 (17)	O23—O22^xviii	2.851 (17)
P—Pb2^viii	4.146 (13)	O23—O22^xiv	3.31 (2)
P—Pb2^ix	4.337 (15)	O23—O23^xxv	4.457 (19)
P—Pb2^xiii	4.249 (15)	O23—O23^xxvi	4.457 (19)
P—P^x	4.241 (16)	O23—O23^xiv	4.19 (3)
P—P^xi	4.317 (17)	O23—O1	2.478 (10)
P—P^xii	4.177 (17)	O23—O1^xi	3.41 (2)
P—P^xiv	3.876 (8)	O23—O1^xii	3.13 (2)
P—O21	1.543 (10)	O1—Pb1^viii	3.11 (3)
P—O21^xv	4.303 (13)	O1—Pb1^ix	3.17 (2)
P—O21^x	4.421 (19)	O1—Pb1^vi	3.221 (18)
P—O21^xi	4.34 (2)	O1—Pb2	2.379 (8)
P—O21^xvi	4.421 (13)	O1—Pb2^x	4.02 (2)
P—O21^xiv	3.57 (2)	O1—Pb2^xi	4.26 (2)
P—O22^xvii	4.389 (14)	O1—Pb2^xii	3.95 (2)
P—O22	1.526 (10)	O1—P	1.511 (7)
P—O22^x	4.30 (2)	O1—P^x	3.36 (2)
P—O22^xii	4.32 (2)	O1—P^xi	3.53 (2)
P—O22^xviii	4.250 (12)	O1—P^xii	3.40 (2)
P—O22^xiv	3.68 (2)	O1—O21	2.493 (11)
P—O23	1.523 (10)	O1—O21^x	3.342 (17)
P—O23^xi	4.400 (19)	O1—O21^xi	3.33 (2)
P—O23^xii	4.153 (19)	O1—O22	2.480 (11)
P—O23^xix	4.423 (18)	O1—O22^x	3.219 (19)
P—O23^xx	4.178 (16)	O1—O22^xii	3.36 (3)
P—O23^xiv	3.735 (17)	O1—O23	2.478 (10)
P—O1	1.511 (7)	O1—O23^xi	3.41 (2)
P—O1^x	3.36 (2)	O1—O23^xii	3.13 (2)
P—O1^xi	3.53 (2)	O1—O1^x	3.03 (4)
P—O1^xii	3.40 (2)	O1—O1^xi	3.30 (4)
O21—Pb1^viii	2.63 (2)	O1—O1^xii	3.20 (4)
O21—Pb1^vi	4.425 (16)
O21—P—O22	109.50 (16)	O22—P—O23	109.46 (15)
O21—P—O23	109.47 (15)	O22—P—O1	109.48 (15)
O21—P—O1	109.45 (16)	O23—P—O1	109.47 (16)

Symmetry codes: (i) z, x, y; (ii) x−1, y−1/2, z+1/2; (iii) x−1, y+1/2, z+1/2; (iv) z, x−1/2, y+1/2; (v) z, x+1/2, y+1/2; (vi) −x, −y+1/2, −z+3/2; (vii) −z−1, −x+1/2, −y+1/2; (viii) x, y−1/2, z+1/2; (ix) x, y+1/2, z+1/2; (x) z+1, x, y; (xi) −x+1, −y, −z+1; (xii) −x+1, −y+1, −z+1; (xiii) −z, −x+1/2, −y+3/2; (xiv) −x+1, −y+1/2, −z+3/2; (xv) x, y+1, z; (xvi) −z, −x, −y+1; (xvii) x, y−1, z; (xviii) −z, −x+1, −y+1; (xix) −z, −x, −y; (xx) −z, −x+1, −y; (xxi) −x+1, −y−1/2, −z+3/2; (xxii) z+1, x−1/2, y+1/2; (xxiii) z+1, x+1/2, y+1/2; (xxiv) −x+1, −y+3/2, −z+3/2; (xxv) z+1, x−1/2, y+3/2; (xxvi) z+1, x+1/2, y+3/2.

(S4P22_phase_1)

Crystal data

O8.00P2Pb3.00	Z = 3
Mr = 811.54	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.4624 (2) Å	Particle morphology: plate
c = 20.0769 (11) Å	irregular, 6 × 6 mm
V = 518.79 (4) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.030	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 71.0 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 9.31 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 120.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 203.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.028	37 parameters
Rexp = 0.016	9 restraints
R(F^2) = 0.20852	(Δ/σ)max = 0.01
χ^2 = 3.062	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 3.17419 2: -0.824729 3: 1.07514 4: -0.199233 5: 0.369686 6: -0.145817 7: 0.229891 8: -0.110337 9: 0.144941 10: -8.808780E-0211: 7.665740E-0212: -1.102230E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92343 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
PB1	0.0	0.0	0.0	0.0195 (15)*
PB2	0.0	0.040 (2)	0.21065 (16)	0.0195 (15)*	0.16667
P	0.0	0.0	0.4037 (3)	0.0109 (13)*
O1	0.0170 (16)	−0.0170 (16)	0.3282 (2)	0.0153 (11)*	0.3333
O2	−0.142 (2)	0.165 (2)	0.42941 (14)	0.0153 (11)*	0.5

Geometric parameters (Å, º)

PB1—PB2	4.235 (3)	P—PB2^lxxii	4.234 (5)
PB1—PB2^i	4.235 (3)	P—PB2^lxxiii	4.090 (9)
PB1—PB2^ii	4.235 (3)	P—PB2^lxxiv	4.374 (8)
PB1—PB2^iii	4.235 (3)	P—PB2^lxxv	4.090 (9)
PB1—PB2^iv	4.235 (3)	P—PB2^lxxvi	4.234 (5)
PB1—PB2^v	4.235 (3)	P—PB2^lxxvii	4.374 (8)
PB1—PB2^vi	4.235 (3)	P—PB2^lxxviii	4.234 (5)
PB1—PB2^vii	4.235 (3)	P—PB2^lxxix	4.374 (8)
PB1—PB2^viii	4.235 (3)	P—PB2^lxxx	4.090 (9)
PB1—PB2^ix	4.235 (3)	P—PB2^lxxxi	4.374 (8)
PB1—PB2^x	4.235 (3)	P—PB2^lxxxii	4.090 (9)
PB1—PB2^xi	4.235 (3)	P—PB2^lxxxiii	4.234 (5)
PB1—PB2^xii	4.008 (2)	P—P^lxxxiv	3.868 (11)
PB1—PB2^xiii	3.855 (7)	P—P^li	4.234 (7)
PB1—PB2^xiv	4.155 (8)	P—P^lii	4.234 (7)
PB1—PB2^xv	4.155 (8)	P—P^liii	4.234 (7)
PB1—PB2^xvi	4.008 (2)	P—O1	1.525 (7)
PB1—PB2^xvii	3.855 (7)	P—O1^i	1.525 (7)
PB1—PB2^xviii	3.855 (7)	P—O1^ii	1.525 (7)
PB1—PB2^xix	4.155 (8)	P—O1^li	3.492 (8)
PB1—PB2^xx	4.008 (2)	P—O1^lii	3.267 (14)
PB1—PB2^xxi	3.855 (7)	P—O1^liii	3.492 (8)
PB1—PB2^xxii	4.008 (2)	P—O1^liv	3.492 (8)
PB1—PB2^xxiii	4.155 (8)	P—O1^lv	3.492 (8)
PB1—PB2^xxiv	4.155 (8)	P—O1^lvi	3.267 (14)
PB1—PB2^xxv	3.855 (7)	P—O1^lvii	3.267 (14)
PB1—PB2^xxvi	4.008 (2)	P—O1^lviii	3.492 (8)
PB1—PB2^xxvii	4.008 (2)	P—O1^lix	3.492 (8)
PB1—PB2^xxviii	4.155 (8)	P—O2^lxxxv	4.260 (8)
PB1—PB2^xxix	3.855 (7)	P—O2	1.540 (4)
PB1—PB2^xxx	4.155 (8)	P—O2^lxxxvi	4.341 (8)
PB1—PB2^xxxi	3.855 (7)	P—O2^i	1.540 (4)
PB1—PB2^xxxii	4.008 (2)	P—O2^lxxxvii	4.341 (8)
PB1—PB2^xxxiii	3.855 (7)	P—O2^lxxxviii	4.260 (8)
PB1—PB2^xxxiv	4.008 (2)	P—O2^lxxxix	4.341 (8)
PB1—PB2^xxxv	4.155 (8)	P—O2^xc	4.260 (8)
PB1—PB2^xxxvi	4.008 (2)	P—O2^ii	1.540 (4)
PB1—PB2^xxxvii	4.155 (8)	P—O2^xci	4.260 (8)
PB1—PB2^xxxviii	3.855 (7)	P—O2^xcii	4.341 (8)
PB1—PB2^xxxix	4.155 (8)	P—O2^iii	1.540 (4)
PB1—PB2^xl	4.008 (2)	P—O2^xciii	4.341 (8)
PB1—PB2^xli	3.855 (7)	P—O2^iv	1.540 (4)
PB1—PB2^xlii	4.008 (2)	P—O2^xciv	4.260 (8)
PB1—PB2^xliii	3.855 (7)	P—O2^v	1.540 (4)
PB1—PB2^xliv	4.155 (8)	P—O2^xcv	4.260 (8)
PB1—PB2^xlv	3.855 (7)	P—O2^xcvi	4.341 (8)
PB1—PB2^xlvi	4.155 (8)	P—O2^lxxxiv	3.652 (6)
PB1—PB2^xlvii	4.008 (2)	P—O2^xcvii	3.652 (6)
PB1—P^xii	3.456 (2)	P—O2^xcviii	3.652 (6)
PB1—P^xiii	3.456 (2)	P—O2^xcix	3.652 (6)
PB1—P^xiv	3.456 (2)	P—O2^100	3.652 (6)
PB1—P^xxx	3.456 (2)	P—O2^101	3.652 (6)
PB1—P^xxxi	3.456 (2)	P—O2^li	4.358 (9)
PB1—P^xxxii	3.456 (2)	P—O2^liii	4.278 (9)
PB1—O1^xii	3.078 (7)	P—O2^liv	4.278 (9)
PB1—O1^xiii	3.316 (15)	P—O2^lv	4.358 (9)
PB1—O1^xiv	3.078 (7)	P—O2^lviii	4.278 (9)
PB1—O1^xv	3.078 (7)	P—O2^lix	4.358 (9)
PB1—O1^xvi	3.078 (7)	P—O2^lx	4.358 (9)
PB1—O1^xvii	3.316 (15)	P—O2^lxi	4.278 (9)
PB1—O1^xviii	3.316 (15)	P—O2^lxii	4.278 (9)
PB1—O1^xix	3.078 (7)	P—O2^lxiii	4.358 (9)
PB1—O1^xx	3.078 (7)	P—O2^lxiv	4.358 (9)
PB1—O1^xxx	3.078 (7)	P—O2^lxv	4.278 (9)
PB1—O1^xxxi	3.316 (15)	O1—PB1^xlviii	3.078 (7)
PB1—O1^xxxii	3.078 (7)	O1—PB1^xlix	3.316 (15)
PB1—O1^xxxiii	3.316 (15)	O1—PB1^l	3.078 (7)
PB1—O1^xxxiv	3.078 (7)	O1—PB2	2.388 (6)
PB1—O1^xxxv	3.078 (7)	O1—PB2^i	2.375 (6)
PB1—O1^xxxvi	3.078 (7)	O1—PB2^ii	2.362 (6)
PB1—O1^xxxvii	3.078 (7)	O1—PB2^iii	2.375 (6)
PB1—O1^xxxviii	3.316 (15)	O1—PB2^iv	2.388 (6)
PB1—O2^xiii	2.575 (3)	O1—PB2^v	2.362 (6)
PB1—O2^xvii	2.575 (3)	O1—PB2^li	4.130 (7)
PB1—O2^xviii	2.575 (3)	O1—PB2^lii	4.091 (13)
PB1—O2^xxi	2.575 (3)	O1—PB2^liii	3.982 (9)
PB1—O2^xxv	2.575 (3)	O1—PB2^liv	3.989 (9)
PB1—O2^xxix	2.575 (3)	O1—PB2^lv	3.949 (12)
PB1—O2^xxxi	2.575 (3)	O1—PB2^lvi	4.280 (11)
PB1—O2^xxxiii	2.575 (3)	O1—PB2^lvii	4.287 (12)
PB1—O2^xxxviii	2.575 (3)	O1—PB2^lviii	3.802 (14)
PB1—O2^xli	2.575 (3)	O1—PB2^lix	4.145 (8)
PB1—O2^xliii	2.575 (3)	O1—PB2^lxvi	4.280 (11)
PB1—O2^xlv	2.575 (3)	O1—PB2^lx	3.949 (12)
PB2—PB1	4.235 (3)	O1—PB2^lxi	3.989 (9)
PB2—PB1^xlviii	4.155 (8)	O1—PB2^lxii	3.982 (9)
PB2—PB1^xlix	3.855 (7)	O1—PB2^lxvii	4.091 (13)
PB2—PB1^l	4.008 (2)	O1—PB2^lxiii	4.130 (7)
PB2—PB2^i	0.381 (19)	O1—PB2^lxiv	4.145 (8)
PB2—PB2^ii	0.381 (19)	O1—PB2^lxv	3.802 (14)
PB2—PB2^iii	0.220 (11)	O1—PB2^lxviii	4.287 (12)
PB2—PB2^iv	0.220 (11)	O1—P	1.525 (7)
PB2—PB2^v	0.44 (2)	O1—P^li	3.492 (8)
PB2—PB2^xxx	3.958 (18)	O1—P^lii	3.267 (14)
PB2—PB2^xxxi	3.295 (15)	O1—P^liii	3.492 (8)
PB2—PB2^xxxii	3.641 (4)	O1—O1^i	0.28 (3)
PB2—PB2^xxxiii	3.621 (3)	O1—O1^ii	0.28 (3)
PB2—PB2^xxxiv	3.451 (8)	O1—O1^li	3.333 (17)
PB2—PB2^xxxv	3.784 (9)	O1—O1^lii	2.84 (3)
PB2—PB2^xxxvi	3.784 (9)	O1—O1^liii	3.333 (17)
PB2—PB2^xxxvii	3.621 (3)	O1—O1^liv	3.321 (15)
PB2—PB2^xxxviii	3.451 (8)	O1—O1^lv	3.084 (7)
PB2—PB2^xxxix	3.952 (17)	O1—O1^lvi	3.084 (7)
PB2—PB2^xl	3.465 (7)	O1—O1^lvii	3.084 (7)
PB2—PB2^xli	3.465 (7)	O1—O1^lviii	3.084 (7)
PB2—PB2^xlii	3.796 (10)	O1—O1^lix	3.321 (15)
PB2—PB2^xliii	3.287 (16)	O1—O2	2.594 (10)
PB2—PB2^xliv	3.796 (10)	O1—O2^i	2.459 (6)
PB2—PB2^xlv	3.615 (3)	O1—O2^ii	2.452 (7)
PB2—PB2^xlvi	3.615 (3)	O1—O2^iii	2.459 (6)
PB2—PB2^xlvii	3.615 (3)	O1—O2^iv	2.594 (10)
PB2—P	3.882 (7)	O1—O2^v	2.452 (7)
PB2—P^xii	4.234 (5)	O1—O2^li	3.350 (11)
PB2—P^xiii	4.374 (8)	O1—O2^liii	3.245 (10)
PB2—P^xiv	4.090 (9)	O1—O2^liv	3.349 (13)
PB2—P^li	3.3314 (18)	O1—O2^lv	3.222 (13)
PB2—P^lii	3.507 (9)	O1—O2^lviii	3.119 (16)
PB2—P^liii	3.146 (9)	O1—O2^lix	3.455 (16)
PB2—O1	2.388 (6)	O1—O2^lx	3.222 (13)
PB2—O1^i	2.362 (6)	O1—O2^lxi	3.349 (13)
PB2—O1^ii	2.375 (6)	O1—O2^lxii	3.245 (10)
PB2—O1^li	4.130 (7)	O1—O2^lxiii	3.350 (11)
PB2—O1^lii	4.091 (13)	O1—O2^lxiv	3.455 (16)
PB2—O1^liii	3.982 (9)	O1—O2^lxv	3.119 (16)
PB2—O1^liv	4.145 (8)	O2—PB1^xlix	2.575 (3)
PB2—O1^lv	4.287 (12)	O2—PB2^li	2.954 (13)
PB2—O1^lvi	3.802 (14)	O2—PB2^liii	2.614 (13)
PB2—O1^lvii	3.949 (12)	O2—PB2^liv	2.632 (15)
PB2—O1^lviii	4.280 (11)	O2—PB2^lvi	2.940 (15)
PB2—O1^lix	3.989 (9)	O2—PB2^lvii	2.970 (13)
PB2—O2^xiii	2.981 (6)	O2—PB2^lix	2.633 (12)
PB2—O2^xvii	2.754 (7)	O2—PB2^lxvi	3.064 (16)
PB2—O2^xviii	2.877 (4)	O2—PB2^lxi	2.509 (16)
PB2—O2^xxi	2.867 (4)	O2—PB2^lxii	2.738 (13)
PB2—O2^xxv	2.985 (6)	O2—PB2^lxiii	2.830 (12)
PB2—O2^xxix	2.759 (7)	O2—PB2^lxiv	2.755 (12)
PB2—O2^li	2.954 (13)	O2—PB2^lxviii	2.847 (13)
PB2—O2^liii	2.614 (13)	O2—PB2^xlix	2.981 (6)
PB2—O2^liv	2.633 (12)	O2—PB2^lxx	2.877 (4)
PB2—O2^lv	2.970 (13)	O2—PB2^lxxiii	2.754 (7)
PB2—O2^lviii	2.940 (15)	O2—PB2^lxxvi	2.867 (4)
PB2—O2^lix	2.632 (15)	O2—PB2^lxxix	2.985 (6)
PB2—O2^lx	3.064 (16)	O2—PB2^lxxxii	2.759 (7)
PB2—O2^lxi	2.509 (16)	O2—P^102	4.341 (8)
PB2—O2^lxii	2.830 (12)	O2—P	1.540 (4)
PB2—O2^lxiii	2.738 (13)	O2—P^103	4.260 (8)
PB2—O2^lxiv	2.755 (12)	O2—P^lxxxiv	3.652 (6)
PB2—O2^lxv	2.847 (13)	O2—P^li	4.358 (9)
P—PB1^xlviii	3.456 (2)	O2—P^liii	4.278 (9)
P—PB1^xlix	3.456 (2)	O2—O1	2.594 (10)
P—PB1^l	3.456 (2)	O2—O1^i	2.452 (7)
P—PB2	3.882 (7)	O2—O1^ii	2.459 (6)
P—PB2^i	3.882 (7)	O2—O1^li	3.350 (11)
P—PB2^ii	3.882 (7)	O2—O1^liii	3.245 (10)
P—PB2^iii	3.882 (7)	O2—O1^liv	3.455 (16)
P—PB2^iv	3.882 (7)	O2—O1^lvi	3.119 (16)
P—PB2^v	3.882 (7)	O2—O1^lvii	3.222 (13)
P—PB2^li	3.3314 (18)	O2—O1^lix	3.349 (13)
P—PB2^lii	3.507 (9)	O2—O2^i	2.513 (6)
P—PB2^liii	3.146 (9)	O2—O2^lxxxvii	2.954 (6)
P—PB2^liv	3.146 (9)	O2—O2^xc	2.954 (6)
P—PB2^lv	3.3314 (18)	O2—O2^ii	2.513 (6)
P—PB2^lvi	3.507 (9)	O2—O2^xcii	3.015 (14)
P—PB2^lvii	3.507 (9)	O2—O2^iii	2.448 (14)
P—PB2^lviii	3.146 (9)	O2—O2^iv	0.13 (2)
P—PB2^lix	3.3314 (18)	O2—O2^v	2.574 (13)
P—PB2^lxvi	3.507 (9)	O2—O2^xcv	2.889 (13)
P—PB2^lx	3.3314 (18)	O2—O2^lxxxiv	4.056 (6)
P—PB2^lxi	3.146 (9)	O2—O2^104	4.263 (15)
P—PB2^lxii	3.146 (9)	O2—O2^xcvii	3.184 (5)
P—PB2^lxvii	3.507 (9)	O2—O2^xcviii	3.184 (5)
P—PB2^lxiii	3.3314 (18)	O2—O2^xcix	3.235 (11)
P—PB2^lxiv	3.3314 (18)	O2—O2^105	4.341 (5)
P—PB2^lxv	3.146 (9)	O2—O2^100	4.054 (6)
P—PB2^lxviii	3.507 (9)	O2—O2^106	4.341 (5)
P—PB2^xlviii	4.090 (9)	O2—O2^101	3.135 (10)
P—PB2^xlix	4.374 (8)	O2—O2^liv	4.218 (5)
P—PB2^l	4.234 (5)	O2—O2^lix	4.218 (5)
P—PB2^lxix	4.374 (8)	O2—O2^lxi	4.175 (10)
P—PB2^lxx	4.234 (5)	O2—O2^lxiv	4.263 (10)
P—PB2^lxxi	4.090 (9)
PB2^i—PB2—PB2^ii	60.0000 (2)	O1^ii—P—O2	106.7 (3)
PB2^i—PB2—PB2^iii	90.0000 (2)	O1^ii—P—O2^i	106.3 (4)
PB2^i—PB2—PB2^iv	30.0	O1^ii—P—O2^ii	115.6 (6)
PB2^i—PB2—PB2^v	30.0	O1^ii—P—O2^iii	115.6 (6)
PB2^ii—PB2—PB2^iii	30.0	O1^ii—P—O2^iv	106.3 (4)
PB2^ii—PB2—PB2^iv	90.0000 (2)	O1^ii—P—O2^v	106.7 (3)
PB2^ii—PB2—PB2^v	30.0	O2—P—O2^i	109.3 (2)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	109.3 (2)
PB2^iii—PB2—PB2^v	60.0000 (2)	O2—P—O2^iii	105.2 (8)
PB2^iv—PB2—PB2^v	60.0000 (2)	O2—P—O2^iv	4.7 (9)
O1—P—O1^i	10.5 (10)	O2—P—O2^v	113.3 (8)
O1—P—O1^ii	10.5 (10)	O2^i—P—O2^ii	109.3 (2)
O1—P—O2	115.6 (6)	O2^i—P—O2^iii	113.3 (8)
O1—P—O2^i	106.7 (3)	O2^i—P—O2^iv	105.2 (8)
O1—P—O2^ii	106.3 (4)	O2^i—P—O2^v	4.7 (9)
O1—P—O2^iii	106.7 (3)	O2^ii—P—O2^iii	4.7 (9)
O1—P—O2^iv	115.6 (6)	O2^ii—P—O2^iv	113.3 (8)
O1—P—O2^v	106.3 (4)	O2^ii—P—O2^v	105.2 (8)
O1^i—P—O1^ii	10.5 (10)	O2^iii—P—O2^iv	109.3 (2)
O1^i—P—O2	106.3 (4)	O2^iii—P—O2^v	109.3 (2)
O1^i—P—O2^i	115.6 (6)	O2^iv—P—O2^v	109.3 (2)
O1^i—P—O2^ii	106.7 (3)	P—O1—O1^i	84.8 (5)
O1^i—P—O2^iii	106.3 (4)	P—O1—O1^ii	84.8 (5)
O1^i—P—O2^iv	106.7 (3)	O1^i—O1—O1^ii	60.0000 (2)
O1^i—P—O2^v	115.6 (6)	P—O2—O2^iv	87.7 (4)

Symmetry codes: (i) −y, x−y, z; (ii) y−x, −x, z; (iii) y−x, y, z; (iv) −y, −x, z; (v) x, x−y, z; (vi) −x, −y, −z; (vii) y, y−x, −z; (viii) x−y, x, −z; (ix) x−y, −y, −z; (x) y, x, −z; (xi) −x, y−x, −z; (xii) x−2/3, y−1/3, z−1/3; (xiii) x+1/3, y−1/3, z−1/3; (xiv) x+1/3, y+2/3, z−1/3; (xv) −y−2/3, x−y−1/3, z−1/3; (xvi) −y+1/3, x−y−1/3, z−1/3; (xvii) −y+1/3, x−y+2/3, z−1/3; (xviii) y−x−2/3, −x−1/3, z−1/3; (xix) y−x+1/3, −x−1/3, z−1/3; (xx) y−x+1/3, −x+2/3, z−1/3; (xxi) y−x−2/3, y−1/3, z−1/3; (xxii) y−x+1/3, y−1/3, z−1/3; (xxiii) y−x+1/3, y+2/3, z−1/3; (xxiv) −y−2/3, −x−1/3, z−1/3; (xxv) −y+1/3, −x−1/3, z−1/3; (xxvi) −y+1/3, −x+2/3, z−1/3; (xxvii) x−2/3, x−y−1/3, z−1/3; (xxviii) x+1/3, x−y−1/3, z−1/3; (xxix) x+1/3, x−y+2/3, z−1/3; (xxx) −x−2/3, −y−1/3, −z+2/3; (xxxi) −x−2/3, −y+2/3, −z+2/3; (xxxii) −x+1/3, −y+2/3, −z+2/3; (xxxiii) y−2/3, y−x−1/3, −z+2/3; (xxxiv) y−2/3, y−x+2/3, −z+2/3; (xxxv) y+1/3, y−x+2/3, −z+2/3; (xxxvi) x−y−2/3, x−1/3, −z+2/3; (xxxvii) x−y−2/3, x+2/3, −z+2/3; (xxxviii) x−y+1/3, x+2/3, −z+2/3; (xxxix) x−y−2/3, −y−1/3, −z+2/3; (xl) x−y−2/3, −y+2/3, −z+2/3; (xli) x−y+1/3, −y+2/3, −z+2/3; (xlii) y−2/3, x−1/3, −z+2/3; (xliii) y−2/3, x+2/3, −z+2/3; (xliv) y+1/3, x+2/3, −z+2/3; (xlv) −x−2/3, y−x−1/3, −z+2/3; (xlvi) −x−2/3, y−x+2/3, −z+2/3; (xlvii) −x+1/3, y−x+2/3, −z+2/3; (xlviii) x−1/3, y−2/3, z+1/3; (xlix) x−1/3, y+1/3, z+1/3; (l) x+2/3, y+1/3, z+1/3; (li) −x−1/3, −y−2/3, −z+1/3; (lii) −x+2/3, −y−2/3, −z+1/3; (liii) −x+2/3, −y+1/3, −z+1/3; (liv) y−1/3, y−x−2/3, −z+1/3; (lv) y+2/3, y−x−2/3, −z+1/3; (lvi) y+2/3, y−x+1/3, −z+1/3; (lvii) x−y−1/3, x−2/3, −z+1/3; (lviii) x−y+2/3, x−2/3, −z+1/3; (lix) x−y+2/3, x+1/3, −z+1/3; (lx) x−y+2/3, −y−2/3, −z+1/3; (lxi) x−y+2/3, −y+1/3, −z+1/3; (lxii) y−1/3, x−2/3, −z+1/3; (lxiii) y+2/3, x+1/3, −z+1/3; (lxiv) −x−1/3, y−x−2/3, −z+1/3; (lxv) −x+2/3, y−x−2/3, −z+1/3; (lxvi) x−y−1/3, −y−2/3, −z+1/3; (lxvii) y+2/3, x−2/3, −z+1/3; (lxviii) −x+2/3, y−x+1/3, −z+1/3; (lxix) −y−1/3, x−y−2/3, z+1/3; (lxx) −y−1/3, x−y+1/3, z+1/3; (lxxi) −y+2/3, x−y+1/3, z+1/3; (lxxii) y−x−1/3, −x−2/3, z+1/3; (lxxiii) y−x−1/3, −x+1/3, z+1/3; (lxxiv) y−x+2/3, −x+1/3, z+1/3; (lxxv) y−x−1/3, y−2/3, z+1/3; (lxxvi) y−x−1/3, y+1/3, z+1/3; (lxxvii) y−x+2/3, y+1/3, z+1/3; (lxxviii) −y−1/3, −x−2/3, z+1/3; (lxxix) −y−1/3, −x+1/3, z+1/3; (lxxx) −y+2/3, −x+1/3, z+1/3; (lxxxi) x−1/3, x−y−2/3, z+1/3; (lxxxii) x−1/3, x−y+1/3, z+1/3; (lxxxiii) x+2/3, x−y+1/3, z+1/3; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) −y, x−y+1, z; (lxxxviii) −y+1, x−y+1, z; (lxxxix) y−x−1, −x−1, z; (xc) y−x−1, −x, z; (xci) y−x−1, y−1, z; (xcii) y−x−1, y, z; (xciii) −y, −x−1, z; (xciv) −y+1, −x, z; (xcv) x, x−y+1, z; (xcvi) x+1, x−y+1, z; (xcvii) y, y−x, −z+1; (xcviii) x−y, x, −z+1; (xcix) x−y, −y, −z+1; (100) y, x, −z+1; (101) −x, y−x, −z+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x, −y+1, −z+1; (105) y−1, x, −z+1; (106) y, x+1, −z+1.

(S4P22_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8987 (5) Å	T = 298 K
c = 2.8295 (8) Å	Particle morphology: Pressure cell anvil material
V = 20.59 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.030	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 71.0 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 9.31 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 120.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 203.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.028	37 parameters
Rexp = 0.016	9 restraints
R(F^2) = 0.20852	(Δ/σ)max = 0.01
χ^2 = 3.062	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 3.17419 2: -0.824729 3: 1.07514 4: -0.199233 5: 0.369686 6: -0.145817 7: 0.229891 8: -0.110337 9: 0.144941 10: -8.808780E-0211: 7.665740E-0212: -1.102230E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92343 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.235 (3)	P—PB2	4.234 (5)
PB1—PB2^i	4.235 (3)	P—PB2	4.090 (9)
PB1—PB2^ii	4.235 (3)	P—PB2	4.374 (8)
PB1—PB2^iii	4.235 (3)	P—PB2	4.090 (9)
PB1—PB2^iv	4.235 (3)	P—PB2	4.234 (5)
PB1—PB2^v	4.235 (3)	P—PB2	4.374 (8)
PB1—PB2	4.235 (3)	P—PB2	4.234 (5)
PB1—PB2	4.235 (3)	P—PB2	4.374 (8)
PB1—PB2	4.235 (3)	P—PB2	4.090 (9)
PB1—PB2	4.235 (3)	P—PB2	4.374 (8)
PB1—PB2	4.235 (3)	P—PB2	4.090 (9)
PB1—PB2	4.235 (3)	P—PB2	4.234 (5)
PB1—PB2	4.008 (2)	P—P	3.868 (11)
PB1—PB2	3.855 (7)	P—P	4.234 (7)
PB1—PB2	4.155 (8)	P—P	4.234 (7)
PB1—PB2	4.155 (8)	P—P	4.234 (7)
PB1—PB2	4.008 (2)	P—O1	1.525 (7)
PB1—PB2	3.855 (7)	P—O1^i	1.525 (7)
PB1—PB2	3.855 (7)	P—O1^ii	1.525 (7)
PB1—PB2	4.155 (8)	P—O1	3.492 (8)
PB1—PB2	4.008 (2)	P—O1	3.267 (14)
PB1—PB2	3.855 (7)	P—O1	3.492 (8)
PB1—PB2	4.008 (2)	P—O1	3.492 (8)
PB1—PB2	4.155 (8)	P—O1	3.492 (8)
PB1—PB2	4.155 (8)	P—O1	3.267 (14)
PB1—PB2	3.855 (7)	P—O1	3.267 (14)
PB1—PB2	4.008 (2)	P—O1	3.492 (8)
PB1—PB2	4.008 (2)	P—O1	3.492 (8)
PB1—PB2	4.155 (8)	P—O2^vi	4.260 (8)
PB1—PB2	3.855 (7)	P—O2	1.540 (4)
PB1—PB2	4.155 (8)	P—O2^vii	4.341 (8)
PB1—PB2	3.855 (7)	P—O2^i	1.540 (4)
PB1—PB2	4.008 (2)	P—O2^viii	4.341 (8)
PB1—PB2	3.855 (7)	P—O2^ix	4.260 (8)
PB1—PB2	4.008 (2)	P—O2^x	4.341 (8)
PB1—PB2	4.155 (8)	P—O2^xi	4.260 (8)
PB1—PB2	4.008 (2)	P—O2^ii	1.540 (4)
PB1—PB2	4.155 (8)	P—O2^xii	4.260 (8)
PB1—PB2	3.855 (7)	P—O2^xiii	4.341 (8)
PB1—PB2	4.155 (8)	P—O2^iii	1.540 (4)
PB1—PB2	4.008 (2)	P—O2^xiv	4.341 (8)
PB1—PB2	3.855 (7)	P—O2^iv	1.540 (4)
PB1—PB2	4.008 (2)	P—O2^xv	4.260 (8)
PB1—PB2	3.855 (7)	P—O2^v	1.540 (4)
PB1—PB2	4.155 (8)	P—O2^xvi	4.260 (8)
PB1—PB2	3.855 (7)	P—O2^xvii	4.341 (8)
PB1—PB2	4.155 (8)	P—O2	3.652 (6)
PB1—PB2	4.008 (2)	P—O2	3.652 (6)
PB1—P	3.456 (2)	P—O2	3.652 (6)
PB1—P	3.456 (2)	P—O2	3.652 (6)
PB1—P	3.456 (2)	P—O2	3.652 (6)
PB1—P	3.456 (2)	P—O2	3.652 (6)
PB1—P	3.456 (2)	P—O2	4.358 (9)
PB1—P	3.456 (2)	P—O2	4.278 (9)
PB1—O1	3.078 (7)	P—O2	4.278 (9)
PB1—O1	3.316 (15)	P—O2	4.358 (9)
PB1—O1	3.078 (7)	P—O2	4.278 (9)
PB1—O1	3.078 (7)	P—O2	4.358 (9)
PB1—O1	3.078 (7)	P—O2	4.358 (9)
PB1—O1	3.316 (15)	P—O2	4.278 (9)
PB1—O1	3.316 (15)	P—O2	4.278 (9)
PB1—O1	3.078 (7)	P—O2	4.358 (9)
PB1—O1	3.078 (7)	P—O2	4.358 (9)
PB1—O1	3.078 (7)	P—O2	4.278 (9)
PB1—O1	3.316 (15)	O1—PB1	3.078 (7)
PB1—O1	3.078 (7)	O1—PB1	3.316 (15)
PB1—O1	3.316 (15)	O1—PB1	3.078 (7)
PB1—O1	3.078 (7)	O1—PB2	2.388 (6)
PB1—O1	3.078 (7)	O1—PB2^i	2.375 (6)
PB1—O1	3.078 (7)	O1—PB2^ii	2.362 (6)
PB1—O1	3.078 (7)	O1—PB2^iii	2.375 (6)
PB1—O1	3.316 (15)	O1—PB2^iv	2.388 (6)
PB1—O2	2.575 (3)	O1—PB2^v	2.362 (6)
PB1—O2	2.575 (3)	O1—PB2	4.130 (7)
PB1—O2	2.575 (3)	O1—PB2	4.091 (13)
PB1—O2	2.575 (3)	O1—PB2	3.982 (9)
PB1—O2	2.575 (3)	O1—PB2	3.989 (9)
PB1—O2	2.575 (3)	O1—PB2	3.949 (12)
PB1—O2	2.575 (3)	O1—PB2	4.280 (11)
PB1—O2	2.575 (3)	O1—PB2	4.287 (12)
PB1—O2	2.575 (3)	O1—PB2	3.802 (14)
PB1—O2	2.575 (3)	O1—PB2	4.145 (8)
PB1—O2	2.575 (3)	O1—PB2	4.280 (11)
PB1—O2	2.575 (3)	O1—PB2	3.949 (12)
PB2—PB1	4.235 (3)	O1—PB2	3.989 (9)
PB2—PB1	4.155 (8)	O1—PB2	3.982 (9)
PB2—PB1	3.855 (7)	O1—PB2	4.091 (13)
PB2—PB1	4.008 (2)	O1—PB2	4.130 (7)
PB2—PB2^i	0.381 (19)	O1—PB2	4.145 (8)
PB2—PB2^ii	0.381 (19)	O1—PB2	3.802 (14)
PB2—PB2^iii	0.220 (11)	O1—PB2	4.287 (12)
PB2—PB2^iv	0.220 (11)	O1—P	1.525 (7)
PB2—PB2^v	0.44 (2)	O1—P	3.492 (8)
PB2—PB2	3.958 (18)	O1—P	3.267 (14)
PB2—PB2	3.295 (15)	O1—P	3.492 (8)
PB2—PB2	3.641 (4)	O1—O1^i	0.28 (3)
PB2—PB2	3.621 (3)	O1—O1^ii	0.28 (3)
PB2—PB2	3.451 (8)	O1—O1	3.333 (17)
PB2—PB2	3.784 (9)	O1—O1	2.84 (3)
PB2—PB2	3.784 (9)	O1—O1	3.333 (17)
PB2—PB2	3.621 (3)	O1—O1	3.321 (15)
PB2—PB2	3.451 (8)	O1—O1	3.084 (7)
PB2—PB2	3.952 (17)	O1—O1	3.084 (7)
PB2—PB2	3.465 (7)	O1—O1	3.084 (7)
PB2—PB2	3.465 (7)	O1—O1	3.084 (7)
PB2—PB2	3.796 (10)	O1—O1	3.321 (15)
PB2—PB2	3.287 (16)	O1—O2	2.594 (10)
PB2—PB2	3.796 (10)	O1—O2^i	2.459 (6)
PB2—PB2	3.615 (3)	O1—O2^ii	2.452 (7)
PB2—PB2	3.615 (3)	O1—O2^iii	2.459 (6)
PB2—PB2	3.615 (3)	O1—O2^iv	2.594 (10)
PB2—P	3.882 (7)	O1—O2^v	2.452 (7)
PB2—P	4.234 (5)	O1—O2	3.350 (11)
PB2—P	4.374 (8)	O1—O2	3.245 (10)
PB2—P	4.090 (9)	O1—O2	3.349 (13)
PB2—P	3.3314 (18)	O1—O2	3.222 (13)
PB2—P	3.507 (9)	O1—O2	3.119 (16)
PB2—P	3.146 (9)	O1—O2	3.455 (16)
PB2—O1	2.388 (6)	O1—O2	3.222 (13)
PB2—O1^i	2.362 (6)	O1—O2	3.349 (13)
PB2—O1^ii	2.375 (6)	O1—O2	3.245 (10)
PB2—O1	4.130 (7)	O1—O2	3.350 (11)
PB2—O1	4.091 (13)	O1—O2	3.455 (16)
PB2—O1	3.982 (9)	O1—O2	3.119 (16)
PB2—O1	4.145 (8)	O2—PB1	2.575 (3)
PB2—O1	4.287 (12)	O2—PB2	2.954 (13)
PB2—O1	3.802 (14)	O2—PB2	2.614 (13)
PB2—O1	3.949 (12)	O2—PB2	2.632 (15)
PB2—O1	4.280 (11)	O2—PB2	2.940 (15)
PB2—O1	3.989 (9)	O2—PB2	2.970 (13)
PB2—O2	2.981 (6)	O2—PB2	2.633 (12)
PB2—O2	2.754 (7)	O2—PB2	3.064 (16)
PB2—O2	2.877 (4)	O2—PB2	2.509 (16)
PB2—O2	2.867 (4)	O2—PB2	2.738 (13)
PB2—O2	2.985 (6)	O2—PB2	2.830 (12)
PB2—O2	2.759 (7)	O2—PB2	2.755 (12)
PB2—O2	2.954 (13)	O2—PB2	2.847 (13)
PB2—O2	2.614 (13)	O2—PB2	2.981 (6)
PB2—O2	2.633 (12)	O2—PB2	2.877 (4)
PB2—O2	2.970 (13)	O2—PB2	2.754 (7)
PB2—O2	2.940 (15)	O2—PB2	2.867 (4)
PB2—O2	2.632 (15)	O2—PB2	2.985 (6)
PB2—O2	3.064 (16)	O2—PB2	2.759 (7)
PB2—O2	2.509 (16)	O2—P^xviii	4.341 (8)
PB2—O2	2.830 (12)	O2—P	1.540 (4)
PB2—O2	2.738 (13)	O2—P^xix	4.260 (8)
PB2—O2	2.755 (12)	O2—P	3.652 (6)
PB2—O2	2.847 (13)	O2—P	4.358 (9)
P—PB1	3.456 (2)	O2—P	4.278 (9)
P—PB1	3.456 (2)	O2—O1	2.594 (10)
P—PB1	3.456 (2)	O2—O1^i	2.452 (7)
P—PB2	3.882 (7)	O2—O1^ii	2.459 (6)
P—PB2^i	3.882 (7)	O2—O1	3.350 (11)
P—PB2^ii	3.882 (7)	O2—O1	3.245 (10)
P—PB2^iii	3.882 (7)	O2—O1	3.455 (16)
P—PB2^iv	3.882 (7)	O2—O1	3.119 (16)
P—PB2^v	3.882 (7)	O2—O1	3.222 (13)
P—PB2	3.3314 (18)	O2—O1	3.349 (13)
P—PB2	3.507 (9)	O2—O2^i	2.513 (6)
P—PB2	3.146 (9)	O2—O2^viii	2.954 (6)
P—PB2	3.146 (9)	O2—O2^xi	2.954 (6)
P—PB2	3.3314 (18)	O2—O2^ii	2.513 (6)
P—PB2	3.507 (9)	O2—O2^xiii	3.015 (14)
P—PB2	3.507 (9)	O2—O2^iii	2.448 (14)
P—PB2	3.146 (9)	O2—O2^iv	0.13 (2)
P—PB2	3.3314 (18)	O2—O2^v	2.574 (13)
P—PB2	3.507 (9)	O2—O2^xvi	2.889 (13)
P—PB2	3.3314 (18)	O2—O2	4.056 (6)
P—PB2	3.146 (9)	O2—O2	4.263 (15)
P—PB2	3.146 (9)	O2—O2	3.184 (5)
P—PB2	3.507 (9)	O2—O2	3.184 (5)
P—PB2	3.3314 (18)	O2—O2	3.235 (11)
P—PB2	3.3314 (18)	O2—O2	4.341 (5)
P—PB2	3.146 (9)	O2—O2	4.054 (6)
P—PB2	3.507 (9)	O2—O2	4.341 (5)
P—PB2	4.090 (9)	O2—O2	3.135 (10)
P—PB2	4.374 (8)	O2—O2	4.218 (5)
P—PB2	4.234 (5)	O2—O2	4.218 (5)
P—PB2	4.374 (8)	O2—O2	4.175 (10)
P—PB2	4.234 (5)	O2—O2	4.263 (10)
P—PB2	4.090 (9)
PB2^i—PB2—PB2^ii	60.0000 (2)	O1^ii—P—O2	106.7 (3)
PB2^i—PB2—PB2^iii	90.0000 (2)	O1^ii—P—O2^i	106.3 (4)
PB2^i—PB2—PB2^iv	30.0	O1^ii—P—O2^ii	115.6 (6)
PB2^i—PB2—PB2^v	30.0	O1^ii—P—O2^iii	115.6 (6)
PB2^ii—PB2—PB2^iii	30.0	O1^ii—P—O2^iv	106.3 (4)
PB2^ii—PB2—PB2^iv	90.0000 (2)	O1^ii—P—O2^v	106.7 (3)
PB2^ii—PB2—PB2^v	30.0	O2—P—O2^i	109.3 (2)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	109.3 (2)
PB2^iii—PB2—PB2^v	60.0000 (2)	O2—P—O2^iii	105.2 (8)
PB2^iv—PB2—PB2^v	60.0000 (2)	O2—P—O2^iv	4.7 (9)
O1—P—O1^i	10.5 (10)	O2—P—O2^v	113.3 (8)
O1—P—O1^ii	10.5 (10)	O2^i—P—O2^ii	109.3 (2)
O1—P—O2	115.6 (6)	O2^i—P—O2^iii	113.3 (8)
O1—P—O2^i	106.7 (3)	O2^i—P—O2^iv	105.2 (8)
O1—P—O2^ii	106.3 (4)	O2^i—P—O2^v	4.7 (9)
O1—P—O2^iii	106.7 (3)	O2^ii—P—O2^iii	4.7 (9)
O1—P—O2^iv	115.6 (6)	O2^ii—P—O2^iv	113.3 (8)
O1—P—O2^v	106.3 (4)	O2^ii—P—O2^v	105.2 (8)
O1^i—P—O1^ii	10.5 (10)	O2^iii—P—O2^iv	109.3 (2)
O1^i—P—O2	106.3 (4)	O2^iii—P—O2^v	109.3 (2)
O1^i—P—O2^i	115.6 (6)	O2^iv—P—O2^v	109.3 (2)
O1^i—P—O2^ii	106.7 (3)	P—O1—O1^i	84.8 (5)
O1^i—P—O2^iii	106.3 (4)	P—O1—O1^ii	84.8 (5)
O1^i—P—O2^iv	106.7 (3)	O1^i—O1—O1^ii	60.0000 (2)
O1^i—P—O2^v	115.6 (6)	P—O2—O2^iv	87.7 (4)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) x, y, −z; (iv) y−x, −x, z; (v) −y, x−y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) y−x, −x+1, −z; (ix) y−x+1, −x+1, −z; (x) −y−1, x−y−1, z; (xi) −y−1, x−y, z; (xii) x−1, y−1, −z; (xiii) x−1, y, −z; (xiv) y−x, −x−1, z; (xv) y−x+1, −x, z; (xvi) −y, x−y+1, −z; (xvii) −y+1, x−y+1, −z; (xviii) x−1, y, z; (xix) x, y+1, z.

(S4P22_phase_3)

Crystal data

Ni	anvil material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5456 (6) Å	Particle morphology: Component of pressure cell, not sample
V = 44.57 (3) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.030	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 71.0 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 9.31 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 120.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 203.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.028	37 parameters
Rexp = 0.016	9 restraints
R(F^2) = 0.20852	(Δ/σ)max = 0.01
χ^2 = 3.062	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 3.17419 2: -0.824729 3: 1.07514 4: -0.199233 5: 0.369686 6: -0.145817 7: 0.229891 8: -0.110337 9: 0.144941 10: -8.808780E-0211: 7.665740E-0212: -1.102230E-02
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92343 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.235 (3)	P—PB2^lxxii	4.234 (5)
PB1—PB2^i	4.235 (3)	P—PB2^lxxiii	4.090 (9)
PB1—PB2^ii	4.235 (3)	P—PB2^lxxiv	4.374 (8)
PB1—PB2^iii	4.235 (3)	P—PB2^lxxv	4.090 (9)
PB1—PB2^iv	4.235 (3)	P—PB2^lxxvi	4.234 (5)
PB1—PB2^v	4.235 (3)	P—PB2^lxxvii	4.374 (8)
PB1—PB2^vi	4.235 (3)	P—PB2^lxxviii	4.234 (5)
PB1—PB2^vii	4.235 (3)	P—PB2^lxxix	4.374 (8)
PB1—PB2^viii	4.235 (3)	P—PB2^lxxx	4.090 (9)
PB1—PB2^ix	4.235 (3)	P—PB2^lxxxi	4.374 (8)
PB1—PB2^x	4.235 (3)	P—PB2^lxxxii	4.090 (9)
PB1—PB2^xi	4.235 (3)	P—PB2^lxxxiii	4.234 (5)
PB1—PB2^xii	4.008 (2)	P—P^lxxxiv	3.868 (11)
PB1—PB2^xiii	3.855 (7)	P—P^li	4.234 (7)
PB1—PB2^xiv	4.155 (8)	P—P^lii	4.234 (7)
PB1—PB2^xv	4.155 (8)	P—P^liii	4.234 (7)
PB1—PB2^xvi	4.008 (2)	P—O1	1.525 (7)
PB1—PB2^xvii	3.855 (7)	P—O1^i	1.525 (7)
PB1—PB2^xviii	3.855 (7)	P—O1^ii	1.525 (7)
PB1—PB2^xix	4.155 (8)	P—O1^li	3.492 (8)
PB1—PB2^xx	4.008 (2)	P—O1^lii	3.267 (14)
PB1—PB2^xxi	3.855 (7)	P—O1^liii	3.492 (8)
PB1—PB2^xxii	4.008 (2)	P—O1^liv	3.492 (8)
PB1—PB2^xxiii	4.155 (8)	P—O1^lv	3.492 (8)
PB1—PB2^xxiv	4.155 (8)	P—O1^lvi	3.267 (14)
PB1—PB2^xxv	3.855 (7)	P—O1^lvii	3.267 (14)
PB1—PB2^xxvi	4.008 (2)	P—O1^lviii	3.492 (8)
PB1—PB2^xxvii	4.008 (2)	P—O1^lix	3.492 (8)
PB1—PB2^xxviii	4.155 (8)	P—O2^lxxxv	4.260 (8)
PB1—PB2^xxix	3.855 (7)	P—O2	1.540 (4)
PB1—PB2^xxx	4.155 (8)	P—O2^lxxxvi	4.341 (8)
PB1—PB2^xxxi	3.855 (7)	P—O2^i	1.540 (4)
PB1—PB2^xxxii	4.008 (2)	P—O2^lxxxvii	4.341 (8)
PB1—PB2^xxxiii	3.855 (7)	P—O2^lxxxviii	4.260 (8)
PB1—PB2^xxxiv	4.008 (2)	P—O2^lxxxix	4.341 (8)
PB1—PB2^xxxv	4.155 (8)	P—O2^xc	4.260 (8)
PB1—PB2^xxxvi	4.008 (2)	P—O2^ii	1.540 (4)
PB1—PB2^xxxvii	4.155 (8)	P—O2^xci	4.260 (8)
PB1—PB2^xxxviii	3.855 (7)	P—O2^xcii	4.341 (8)
PB1—PB2^xxxix	4.155 (8)	P—O2^iii	1.540 (4)
PB1—PB2^xl	4.008 (2)	P—O2^xciii	4.341 (8)
PB1—PB2^xli	3.855 (7)	P—O2^iv	1.540 (4)
PB1—PB2^xlii	4.008 (2)	P—O2^xciv	4.260 (8)
PB1—PB2^xliii	3.855 (7)	P—O2^v	1.540 (4)
PB1—PB2^xliv	4.155 (8)	P—O2^xcv	4.260 (8)
PB1—PB2^xlv	3.855 (7)	P—O2^xcvi	4.341 (8)
PB1—PB2^xlvi	4.155 (8)	P—O2^lxxxiv	3.652 (6)
PB1—PB2^xlvii	4.008 (2)	P—O2^xcvii	3.652 (6)
PB1—P^xii	3.456 (2)	P—O2^xcviii	3.652 (6)
PB1—P^xiii	3.456 (2)	P—O2^xcix	3.652 (6)
PB1—P^xiv	3.456 (2)	P—O2^100	3.652 (6)
PB1—P^xxx	3.456 (2)	P—O2^101	3.652 (6)
PB1—P^xxxi	3.456 (2)	P—O2^li	4.358 (9)
PB1—P^xxxii	3.456 (2)	P—O2^liii	4.278 (9)
PB1—O1^xii	3.078 (7)	P—O2^liv	4.278 (9)
PB1—O1^xiii	3.316 (15)	P—O2^lv	4.358 (9)
PB1—O1^xiv	3.078 (7)	P—O2^lviii	4.278 (9)
PB1—O1^xv	3.078 (7)	P—O2^lix	4.358 (9)
PB1—O1^xvi	3.078 (7)	P—O2^lx	4.358 (9)
PB1—O1^xvii	3.316 (15)	P—O2^lxi	4.278 (9)
PB1—O1^xviii	3.316 (15)	P—O2^lxii	4.278 (9)
PB1—O1^xix	3.078 (7)	P—O2^lxiii	4.358 (9)
PB1—O1^xx	3.078 (7)	P—O2^lxiv	4.358 (9)
PB1—O1^xxx	3.078 (7)	P—O2^lxv	4.278 (9)
PB1—O1^xxxi	3.316 (15)	O1—PB1^xlviii	3.078 (7)
PB1—O1^xxxii	3.078 (7)	O1—PB1^xlix	3.316 (15)
PB1—O1^xxxiii	3.316 (15)	O1—PB1^l	3.078 (7)
PB1—O1^xxxiv	3.078 (7)	O1—PB2	2.388 (6)
PB1—O1^xxxv	3.078 (7)	O1—PB2^i	2.375 (6)
PB1—O1^xxxvi	3.078 (7)	O1—PB2^ii	2.362 (6)
PB1—O1^xxxvii	3.078 (7)	O1—PB2^iii	2.375 (6)
PB1—O1^xxxviii	3.316 (15)	O1—PB2^iv	2.388 (6)
PB1—O2^xiii	2.575 (3)	O1—PB2^v	2.362 (6)
PB1—O2^xvii	2.575 (3)	O1—PB2^li	4.130 (7)
PB1—O2^xviii	2.575 (3)	O1—PB2^lii	4.091 (13)
PB1—O2^xxi	2.575 (3)	O1—PB2^liii	3.982 (9)
PB1—O2^xxv	2.575 (3)	O1—PB2^liv	3.989 (9)
PB1—O2^xxix	2.575 (3)	O1—PB2^lv	3.949 (12)
PB1—O2^xxxi	2.575 (3)	O1—PB2^lvi	4.280 (11)
PB1—O2^xxxiii	2.575 (3)	O1—PB2^lvii	4.287 (12)
PB1—O2^xxxviii	2.575 (3)	O1—PB2^lviii	3.802 (14)
PB1—O2^xli	2.575 (3)	O1—PB2^lix	4.145 (8)
PB1—O2^xliii	2.575 (3)	O1—PB2^lxvi	4.280 (11)
PB1—O2^xlv	2.575 (3)	O1—PB2^lx	3.949 (12)
PB2—PB1	4.235 (3)	O1—PB2^lxi	3.989 (9)
PB2—PB1^xlviii	4.155 (8)	O1—PB2^lxii	3.982 (9)
PB2—PB1^xlix	3.855 (7)	O1—PB2^lxvii	4.091 (13)
PB2—PB1^l	4.008 (2)	O1—PB2^lxiii	4.130 (7)
PB2—PB2^i	0.381 (19)	O1—PB2^lxiv	4.145 (8)
PB2—PB2^ii	0.381 (19)	O1—PB2^lxv	3.802 (14)
PB2—PB2^iii	0.220 (11)	O1—PB2^lxviii	4.287 (12)
PB2—PB2^iv	0.220 (11)	O1—P	1.525 (7)
PB2—PB2^v	0.44 (2)	O1—P^li	3.492 (8)
PB2—PB2^xxx	3.958 (18)	O1—P^lii	3.267 (14)
PB2—PB2^xxxi	3.295 (15)	O1—P^liii	3.492 (8)
PB2—PB2^xxxii	3.641 (4)	O1—O1^i	0.28 (3)
PB2—PB2^xxxiii	3.621 (3)	O1—O1^ii	0.28 (3)
PB2—PB2^xxxiv	3.451 (8)	O1—O1^li	3.333 (17)
PB2—PB2^xxxv	3.784 (9)	O1—O1^lii	2.84 (3)
PB2—PB2^xxxvi	3.784 (9)	O1—O1^liii	3.333 (17)
PB2—PB2^xxxvii	3.621 (3)	O1—O1^liv	3.321 (15)
PB2—PB2^xxxviii	3.451 (8)	O1—O1^lv	3.084 (7)
PB2—PB2^xxxix	3.952 (17)	O1—O1^lvi	3.084 (7)
PB2—PB2^xl	3.465 (7)	O1—O1^lvii	3.084 (7)
PB2—PB2^xli	3.465 (7)	O1—O1^lviii	3.084 (7)
PB2—PB2^xlii	3.796 (10)	O1—O1^lix	3.321 (15)
PB2—PB2^xliii	3.287 (16)	O1—O2	2.594 (10)
PB2—PB2^xliv	3.796 (10)	O1—O2^i	2.459 (6)
PB2—PB2^xlv	3.615 (3)	O1—O2^ii	2.452 (7)
PB2—PB2^xlvi	3.615 (3)	O1—O2^iii	2.459 (6)
PB2—PB2^xlvii	3.615 (3)	O1—O2^iv	2.594 (10)
PB2—P	3.882 (7)	O1—O2^v	2.452 (7)
PB2—P^xii	4.234 (5)	O1—O2^li	3.350 (11)
PB2—P^xiii	4.374 (8)	O1—O2^liii	3.245 (10)
PB2—P^xiv	4.090 (9)	O1—O2^liv	3.349 (13)
PB2—P^li	3.3314 (18)	O1—O2^lv	3.222 (13)
PB2—P^lii	3.507 (9)	O1—O2^lviii	3.119 (16)
PB2—P^liii	3.146 (9)	O1—O2^lix	3.455 (16)
PB2—O1	2.388 (6)	O1—O2^lx	3.222 (13)
PB2—O1^i	2.362 (6)	O1—O2^lxi	3.349 (13)
PB2—O1^ii	2.375 (6)	O1—O2^lxii	3.245 (10)
PB2—O1^li	4.130 (7)	O1—O2^lxiii	3.350 (11)
PB2—O1^lii	4.091 (13)	O1—O2^lxiv	3.455 (16)
PB2—O1^liii	3.982 (9)	O1—O2^lxv	3.119 (16)
PB2—O1^liv	4.145 (8)	O2—PB1^xlix	2.575 (3)
PB2—O1^lv	4.287 (12)	O2—PB2^li	2.954 (13)
PB2—O1^lvi	3.802 (14)	O2—PB2^liii	2.614 (13)
PB2—O1^lvii	3.949 (12)	O2—PB2^liv	2.632 (15)
PB2—O1^lviii	4.280 (11)	O2—PB2^lvi	2.940 (15)
PB2—O1^lix	3.989 (9)	O2—PB2^lvii	2.970 (13)
PB2—O2^xiii	2.981 (6)	O2—PB2^lix	2.633 (12)
PB2—O2^xvii	2.754 (7)	O2—PB2^lxvi	3.064 (16)
PB2—O2^xviii	2.877 (4)	O2—PB2^lxi	2.509 (16)
PB2—O2^xxi	2.867 (4)	O2—PB2^lxii	2.738 (13)
PB2—O2^xxv	2.985 (6)	O2—PB2^lxiii	2.830 (12)
PB2—O2^xxix	2.759 (7)	O2—PB2^lxiv	2.755 (12)
PB2—O2^li	2.954 (13)	O2—PB2^lxviii	2.847 (13)
PB2—O2^liii	2.614 (13)	O2—PB2^xlix	2.981 (6)
PB2—O2^liv	2.633 (12)	O2—PB2^lxx	2.877 (4)
PB2—O2^lv	2.970 (13)	O2—PB2^lxxiii	2.754 (7)
PB2—O2^lviii	2.940 (15)	O2—PB2^lxxvi	2.867 (4)
PB2—O2^lix	2.632 (15)	O2—PB2^lxxix	2.985 (6)
PB2—O2^lx	3.064 (16)	O2—PB2^lxxxii	2.759 (7)
PB2—O2^lxi	2.509 (16)	O2—P^102	4.341 (8)
PB2—O2^lxii	2.830 (12)	O2—P	1.540 (4)
PB2—O2^lxiii	2.738 (13)	O2—P^103	4.260 (8)
PB2—O2^lxiv	2.755 (12)	O2—P^lxxxiv	3.652 (6)
PB2—O2^lxv	2.847 (13)	O2—P^li	4.358 (9)
P—PB1^xlviii	3.456 (2)	O2—P^liii	4.278 (9)
P—PB1^xlix	3.456 (2)	O2—O1	2.594 (10)
P—PB1^l	3.456 (2)	O2—O1^i	2.452 (7)
P—PB2	3.882 (7)	O2—O1^ii	2.459 (6)
P—PB2^i	3.882 (7)	O2—O1^li	3.350 (11)
P—PB2^ii	3.882 (7)	O2—O1^liii	3.245 (10)
P—PB2^iii	3.882 (7)	O2—O1^liv	3.455 (16)
P—PB2^iv	3.882 (7)	O2—O1^lvi	3.119 (16)
P—PB2^v	3.882 (7)	O2—O1^lvii	3.222 (13)
P—PB2^li	3.3314 (18)	O2—O1^lix	3.349 (13)
P—PB2^lii	3.507 (9)	O2—O2^i	2.513 (6)
P—PB2^liii	3.146 (9)	O2—O2^lxxxvii	2.954 (6)
P—PB2^liv	3.146 (9)	O2—O2^xc	2.954 (6)
P—PB2^lv	3.3314 (18)	O2—O2^ii	2.513 (6)
P—PB2^lvi	3.507 (9)	O2—O2^xcii	3.015 (14)
P—PB2^lvii	3.507 (9)	O2—O2^iii	2.448 (14)
P—PB2^lviii	3.146 (9)	O2—O2^iv	0.13 (2)
P—PB2^lix	3.3314 (18)	O2—O2^v	2.574 (13)
P—PB2^lxvi	3.507 (9)	O2—O2^xcv	2.889 (13)
P—PB2^lx	3.3314 (18)	O2—O2^lxxxiv	4.056 (6)
P—PB2^lxi	3.146 (9)	O2—O2^104	4.263 (15)
P—PB2^lxii	3.146 (9)	O2—O2^xcvii	3.184 (5)
P—PB2^lxvii	3.507 (9)	O2—O2^xcviii	3.184 (5)
P—PB2^lxiii	3.3314 (18)	O2—O2^xcix	3.235 (11)
P—PB2^lxiv	3.3314 (18)	O2—O2^105	4.341 (5)
P—PB2^lxv	3.146 (9)	O2—O2^100	4.054 (6)
P—PB2^lxviii	3.507 (9)	O2—O2^106	4.341 (5)
P—PB2^xlviii	4.090 (9)	O2—O2^101	3.135 (10)
P—PB2^xlix	4.374 (8)	O2—O2^liv	4.218 (5)
P—PB2^l	4.234 (5)	O2—O2^lix	4.218 (5)
P—PB2^lxix	4.374 (8)	O2—O2^lxi	4.175 (10)
P—PB2^lxx	4.234 (5)	O2—O2^lxiv	4.263 (10)
P—PB2^lxxi	4.090 (9)
PB2^i—PB2—PB2^ii	60.0000 (2)	O1^ii—P—O2	106.7 (3)
PB2^i—PB2—PB2^iii	90.0000 (2)	O1^ii—P—O2^i	106.3 (4)
PB2^i—PB2—PB2^iv	30.0	O1^ii—P—O2^ii	115.6 (6)
PB2^i—PB2—PB2^v	30.0	O1^ii—P—O2^iii	115.6 (6)
PB2^ii—PB2—PB2^iii	30.0	O1^ii—P—O2^iv	106.3 (4)
PB2^ii—PB2—PB2^iv	90.0000 (2)	O1^ii—P—O2^v	106.7 (3)
PB2^ii—PB2—PB2^v	30.0	O2—P—O2^i	109.3 (2)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	109.3 (2)
PB2^iii—PB2—PB2^v	60.0000 (2)	O2—P—O2^iii	105.2 (8)
PB2^iv—PB2—PB2^v	60.0000 (2)	O2—P—O2^iv	4.7 (9)
O1—P—O1^i	10.5 (10)	O2—P—O2^v	113.3 (8)
O1—P—O1^ii	10.5 (10)	O2^i—P—O2^ii	109.3 (2)
O1—P—O2	115.6 (6)	O2^i—P—O2^iii	113.3 (8)
O1—P—O2^i	106.7 (3)	O2^i—P—O2^iv	105.2 (8)
O1—P—O2^ii	106.3 (4)	O2^i—P—O2^v	4.7 (9)
O1—P—O2^iii	106.7 (3)	O2^ii—P—O2^iii	4.7 (9)
O1—P—O2^iv	115.6 (6)	O2^ii—P—O2^iv	113.3 (8)
O1—P—O2^v	106.3 (4)	O2^ii—P—O2^v	105.2 (8)
O1^i—P—O1^ii	10.5 (10)	O2^iii—P—O2^iv	109.3 (2)
O1^i—P—O2	106.3 (4)	O2^iii—P—O2^v	109.3 (2)
O1^i—P—O2^i	115.6 (6)	O2^iv—P—O2^v	109.3 (2)
O1^i—P—O2^ii	106.7 (3)	P—O1—O1^i	84.8 (5)
O1^i—P—O2^iii	106.3 (4)	P—O1—O1^ii	84.8 (5)
O1^i—P—O2^iv	106.7 (3)	O1^i—O1—O1^ii	60.0000 (2)
O1^i—P—O2^v	115.6 (6)	P—O2—O2^iv	87.7 (4)

Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) x, y, −z; (iv) −z, x, y; (v) y, −z, x; (vi) −x, −y, −z; (vii) −z, −x, −y; (viii) −y, −z, −x; (ix) −x, −y, z; (x) z, −x, −y; (xi) −y, z, −x; (xii) x−1, y−1/2, z−1/2; (xiii) x, y−1/2, z−1/2; (xiv) x, y+1/2, z−1/2; (xv) z−1, x−1/2, y−1/2; (xvi) z, x−1/2, y−1/2; (xvii) z, x+1/2, y−1/2; (xviii) y−1, z−1/2, x−1/2; (xix) y, z−1/2, x−1/2; (xx) y, z+1/2, x−1/2; (xxi) x−1, y−1/2, −z−1/2; (xxii) x, y−1/2, −z−1/2; (xxiii) x, y+1/2, −z−1/2; (xxiv) −z−1, x−1/2, y−1/2; (xxv) −z, x−1/2, y−1/2; (xxvi) −z, x+1/2, y−1/2; (xxvii) y−1, −z−1/2, x−1/2; (xxviii) y, −z−1/2, x−1/2; (xxix) y, −z+1/2, x−1/2; (xxx) −x−1/2, −y−1, −z+1/2; (xxxi) −x−1/2, −y, −z+1/2; (xxxii) −x+1/2, −y, −z+1/2; (xxxiii) −z−1/2, −x−1, −y+1/2; (xxxiv) −z−1/2, −x, −y+1/2; (xxxv) −z+1/2, −x, −y+1/2; (xxxvi) −y−1/2, −z−1, −x+1/2; (xxxvii) −y−1/2, −z, −x+1/2; (xxxviii) −y+1/2, −z, −x+1/2; (xxxix) −x−1/2, −y−1, z+1/2; (xl) −x−1/2, −y, z+1/2; (xli) −x+1/2, −y, z+1/2; (xlii) z−1/2, −x−1, −y+1/2; (xliii) z−1/2, −x, −y+1/2; (xliv) z+1/2, −x, −y+1/2; (xlv) −y−1/2, z−1, −x+1/2; (xlvi) −y−1/2, z, −x+1/2; (xlvii) −y+1/2, z, −x+1/2; (xlviii) x−1/2, y−1, z+1/2; (xlix) x−1/2, y, z+1/2; (l) x+1/2, y, z+1/2; (li) −x−1, −y−1/2, −z+1/2; (lii) −x, −y−1/2, −z+1/2; (liii) −x, −y+1/2, −z+1/2; (liv) −z−1, −x−1/2, −y+1/2; (lv) −z, −x−1/2, −y+1/2; (lvi) −z, −x+1/2, −y+1/2; (lvii) −y−1, −z−1/2, −x+1/2; (lviii) −y, −z−1/2, −x+1/2; (lix) −y, −z+1/2, −x+1/2; (lx) −x, −y−1/2, z+1/2; (lxi) −x, −y+1/2, z+1/2; (lxii) z−1, −x−1/2, −y+1/2; (lxiii) z, −x+1/2, −y+1/2; (lxiv) −y−1, z−1/2, −x+1/2; (lxv) −y, z−1/2, −x+1/2; (lxvi) −x−1, −y−1/2, z+1/2; (lxvii) z, −x−1/2, −y+1/2; (lxviii) −y, z+1/2, −x+1/2; (lxix) z−1/2, x−1, y+1/2; (lxx) z−1/2, x, y+1/2; (lxxi) z+1/2, x, y+1/2; (lxxii) y−1/2, z−1, x+1/2; (lxxiii) y−1/2, z, x+1/2; (lxxiv) y+1/2, z, x+1/2; (lxxv) x−1/2, y−1, −z+1/2; (lxxvi) x−1/2, y, −z+1/2; (lxxvii) x+1/2, y, −z+1/2; (lxxviii) −z−1/2, x−1, y+1/2; (lxxix) −z−1/2, x, y+1/2; (lxxx) −z+1/2, x, y+1/2; (lxxxi) y−1/2, −z−1, x+1/2; (lxxxii) y−1/2, −z, x+1/2; (lxxxiii) y+1/2, −z, x+1/2; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) z, x+1, y; (lxxxviii) z+1, x+1, y; (lxxxix) y−1, z−1, x; (xc) y−1, z, x; (xci) x−1, y−1, −z; (xcii) x−1, y, −z; (xciii) −z, x−1, y; (xciv) −z+1, x, y; (xcv) y, −z+1, x; (xcvi) y+1, −z+1, x; (xcvii) −z, −x, −y+1; (xcviii) −y, −z, −x+1; (xcix) −x, −y, z+1; (100) z, −x, −y+1; (101) −y, z, −x+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x, −y+1, −z+1; (105) z−1, −x, −y+1; (106) z, −x+1, −y+1.

(S4P29_phase_1)

Crystal data

O8.00P2Pb3.00	Z = 3
Mr = 811.54	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.4415 (3) Å	Particle morphology: plate
c = 20.0312 (14) Å	irregular, 6 × 6 mm
V = 513.66 (5) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.042	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 80.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 7.51 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 131.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 275.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	37 parameters
Rexp = 0.026	9 restraints
R(F^2) = 0.20098	(Δ/σ)max = 0.07
χ^2 = 1.769	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.85806 2: -0.416774 3: 0.618934 4: -7.414880E-02 5: 0.229918 6: -8.061570E-02 7: 0.156447 8: -5.782420E-02 9: 8.559980E-0210: -3.797140E-0211: 4.114650E-0212: 5.205830E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92661 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
PB1	0.0	0.0	0.0	0.0222 (18)*
PB2	0.0	0.034 (3)	0.21016 (19)	0.0222 (18)*	0.16667
P	0.0	0.0	0.4039 (3)	0.0094 (15)*
O1	0.016 (2)	−0.016 (2)	0.3284 (3)	0.0166 (13)*	0.3333
O2	−0.149 (2)	0.158 (2)	0.42964 (17)	0.0166 (13)*	0.5

Geometric parameters (Å, º)

PB1—PB2	4.214 (4)	P—PB2^lxxii	4.210 (5)
PB1—PB2^i	4.214 (4)	P—PB2^lxxiii	4.089 (11)
PB1—PB2^ii	4.214 (4)	P—PB2^lxxiv	4.328 (11)
PB1—PB2^iii	4.214 (4)	P—PB2^lxxv	4.089 (11)
PB1—PB2^iv	4.214 (4)	P—PB2^lxxvi	4.210 (5)
PB1—PB2^v	4.214 (4)	P—PB2^lxxvii	4.328 (11)
PB1—PB2^vi	4.214 (4)	P—PB2^lxxviii	4.210 (5)
PB1—PB2^vii	4.214 (4)	P—PB2^lxxix	4.328 (11)
PB1—PB2^viii	4.214 (4)	P—PB2^lxxx	4.089 (11)
PB1—PB2^ix	4.214 (4)	P—PB2^lxxxi	4.328 (11)
PB1—PB2^x	4.214 (4)	P—PB2^lxxxii	4.089 (11)
PB1—PB2^xi	4.214 (4)	P—PB2^lxxxiii	4.210 (5)
PB1—PB2^xii	3.999 (2)	P—P^lxxxiv	3.850 (11)
PB1—PB2^xiii	3.871 (10)	P—P^li	4.226 (8)
PB1—PB2^xiv	4.122 (11)	P—P^lii	4.226 (8)
PB1—PB2^xv	4.122 (11)	P—P^liii	4.226 (8)
PB1—PB2^xvi	3.999 (2)	P—O1	1.520 (6)
PB1—PB2^xvii	3.871 (10)	P—O1^i	1.520 (6)
PB1—PB2^xviii	3.871 (10)	P—O1^ii	1.520 (6)
PB1—PB2^xix	4.122 (11)	P—O1^li	3.475 (10)
PB1—PB2^xx	3.999 (2)	P—O1^lii	3.271 (17)
PB1—PB2^xxi	3.871 (10)	P—O1^liii	3.475 (10)
PB1—PB2^xxii	3.999 (2)	P—O1^liv	3.475 (10)
PB1—PB2^xxiii	4.122 (11)	P—O1^lv	3.475 (10)
PB1—PB2^xxiv	4.122 (11)	P—O1^lvi	3.271 (17)
PB1—PB2^xxv	3.871 (10)	P—O1^lvii	3.271 (17)
PB1—PB2^xxvi	3.999 (2)	P—O1^lviii	3.475 (10)
PB1—PB2^xxvii	3.999 (2)	P—O1^lix	3.475 (10)
PB1—PB2^xxviii	4.122 (11)	P—O2^lxxxv	4.265 (8)
PB1—PB2^xxix	3.871 (10)	P—O2	1.537 (4)
PB1—PB2^xxx	4.122 (11)	P—O2^lxxxvi	4.297 (8)
PB1—PB2^xxxi	3.871 (10)	P—O2^i	1.537 (4)
PB1—PB2^xxxii	3.999 (2)	P—O2^lxxxvii	4.297 (8)
PB1—PB2^xxxiii	3.871 (10)	P—O2^lxxxviii	4.265 (8)
PB1—PB2^xxxiv	3.999 (2)	P—O2^lxxxix	4.297 (8)
PB1—PB2^xxxv	4.122 (11)	P—O2^xc	4.265 (8)
PB1—PB2^xxxvi	3.999 (2)	P—O2^ii	1.537 (4)
PB1—PB2^xxxvii	4.122 (11)	P—O2^xci	4.265 (8)
PB1—PB2^xxxviii	3.871 (10)	P—O2^xcii	4.297 (8)
PB1—PB2^xxxix	4.122 (11)	P—O2^iii	1.537 (4)
PB1—PB2^xl	3.999 (2)	P—O2^xciii	4.297 (8)
PB1—PB2^xli	3.871 (10)	P—O2^iv	1.537 (4)
PB1—PB2^xlii	3.999 (2)	P—O2^xciv	4.265 (8)
PB1—PB2^xliii	3.871 (10)	P—O2^v	1.537 (4)
PB1—PB2^xliv	4.122 (11)	P—O2^xcv	4.265 (8)
PB1—PB2^xlv	3.871 (10)	P—O2^xcvi	4.297 (8)
PB1—PB2^xlvi	4.122 (11)	P—O2^lxxxiv	3.635 (6)
PB1—PB2^xlvii	3.999 (2)	P—O2^xcvii	3.635 (6)
PB1—P^xii	3.445 (2)	P—O2^xcviii	3.635 (6)
PB1—P^xiii	3.445 (2)	P—O2^xcix	3.635 (6)
PB1—P^xiv	3.445 (2)	P—O2^100	3.635 (6)
PB1—P^xxx	3.445 (2)	P—O2^101	3.635 (6)
PB1—P^xxxi	3.445 (2)	P—O2^li	4.327 (9)
PB1—P^xxxii	3.445 (2)	P—O2^liii	4.296 (9)
PB1—O1^xii	3.073 (9)	P—O2^liv	4.296 (9)
PB1—O1^xiii	3.290 (18)	P—O2^lv	4.327 (9)
PB1—O1^xiv	3.073 (9)	P—O2^lviii	4.296 (9)
PB1—O1^xv	3.073 (9)	P—O2^lix	4.327 (9)
PB1—O1^xvi	3.073 (9)	P—O2^lx	4.327 (9)
PB1—O1^xvii	3.290 (18)	P—O2^lxi	4.296 (9)
PB1—O1^xviii	3.290 (18)	P—O2^lxii	4.296 (9)
PB1—O1^xix	3.073 (9)	P—O2^lxiii	4.327 (9)
PB1—O1^xx	3.073 (9)	P—O2^lxiv	4.327 (9)
PB1—O1^xxx	3.073 (9)	P—O2^lxv	4.296 (9)
PB1—O1^xxxi	3.290 (18)	O1—PB1^xlviii	3.073 (9)
PB1—O1^xxxii	3.073 (9)	O1—PB1^xlix	3.290 (18)
PB1—O1^xxxiii	3.290 (18)	O1—PB1^l	3.073 (9)
PB1—O1^xxxiv	3.073 (9)	O1—PB2	2.389 (7)
PB1—O1^xxxv	3.073 (9)	O1—PB2^i	2.379 (7)
PB1—O1^xxxvi	3.073 (9)	O1—PB2^ii	2.369 (7)
PB1—O1^xxxvii	3.073 (9)	O1—PB2^iii	2.379 (7)
PB1—O1^xxxviii	3.290 (18)	O1—PB2^iv	2.389 (7)
PB1—O2^xiii	2.567 (4)	O1—PB2^v	2.369 (7)
PB1—O2^xvii	2.567 (4)	O1—PB2^li	4.114 (8)
PB1—O2^xviii	2.567 (4)	O1—PB2^lii	4.068 (17)
PB1—O2^xxi	2.567 (4)	O1—PB2^liii	3.991 (12)
PB1—O2^xxv	2.567 (4)	O1—PB2^liv	3.996 (12)
PB1—O2^xxix	2.567 (4)	O1—PB2^lv	3.949 (14)
PB1—O2^xxxi	2.567 (4)	O1—PB2^lvi	4.240 (14)
PB1—O2^xxxiii	2.567 (4)	O1—PB2^lvii	4.246 (15)
PB1—O2^xxxviii	2.567 (4)	O1—PB2^lviii	3.826 (18)
PB1—O2^xli	2.567 (4)	O1—PB2^lix	4.126 (10)
PB1—O2^xliii	2.567 (4)	O1—PB2^lxvi	4.240 (14)
PB1—O2^xlv	2.567 (4)	O1—PB2^lx	3.949 (14)
PB2—PB1	4.214 (4)	O1—PB2^lxi	3.996 (12)
PB2—PB1^xlviii	4.122 (11)	O1—PB2^lxii	3.991 (12)
PB2—PB1^xlix	3.871 (10)	O1—PB2^lxvii	4.068 (17)
PB2—PB1^l	3.999 (2)	O1—PB2^lxiii	4.114 (8)
PB2—PB2^i	0.32 (3)	O1—PB2^lxiv	4.126 (10)
PB2—PB2^ii	0.32 (3)	O1—PB2^lxv	3.826 (18)
PB2—PB2^iii	0.184 (15)	O1—PB2^lxviii	4.246 (15)
PB2—PB2^iv	0.184 (15)	O1—P	1.520 (6)
PB2—PB2^v	0.37 (3)	O1—P^li	3.475 (10)
PB2—PB2^xxx	3.88 (3)	O1—P^lii	3.271 (17)
PB2—PB2^xxxi	3.32 (2)	O1—P^liii	3.475 (10)
PB2—PB2^xxxii	3.611 (5)	O1—O1^i	0.25 (3)
PB2—PB2^xxxiii	3.597 (4)	O1—O1^ii	0.25 (3)
PB2—PB2^xxxiv	3.455 (12)	O1—O1^li	3.30 (2)
PB2—PB2^xxxv	3.734 (13)	O1—O1^lii	2.86 (4)
PB2—PB2^xxxvi	3.734 (13)	O1—O1^liii	3.30 (2)
PB2—PB2^xxxvii	3.597 (4)	O1—O1^liv	3.294 (18)
PB2—PB2^xxxviii	3.455 (12)	O1—O1^lv	3.077 (9)
PB2—PB2^xxxix	3.88 (2)	O1—O1^lvi	3.077 (9)
PB2—PB2^xl	3.465 (10)	O1—O1^lvii	3.077 (9)
PB2—PB2^xli	3.465 (10)	O1—O1^lviii	3.077 (9)
PB2—PB2^xlii	3.743 (14)	O1—O1^lix	3.294 (18)
PB2—PB2^xliii	3.32 (2)	O1—O2	2.580 (12)
PB2—PB2^xliv	3.743 (14)	O1—O2^i	2.455 (7)
PB2—PB2^xlv	3.593 (4)	O1—O2^ii	2.453 (7)
PB2—PB2^xlvi	3.593 (4)	O1—O2^iii	2.455 (7)
PB2—PB2^xlvii	3.593 (4)	O1—O2^iv	2.580 (12)
PB2—P	3.885 (8)	O1—O2^v	2.453 (7)
PB2—P^xii	4.210 (5)	O1—O2^li	3.310 (10)
PB2—P^xiii	4.328 (11)	O1—O2^liii	3.269 (10)
PB2—P^xiv	4.089 (11)	O1—O2^liv	3.364 (16)
PB2—P^li	3.3189 (19)	O1—O2^lv	3.195 (16)
PB2—P^lii	3.467 (13)	O1—O2^lviii	3.154 (17)
PB2—P^liii	3.164 (13)	O1—O2^lix	3.406 (17)
PB2—O1	2.389 (7)	O1—O2^lx	3.195 (16)
PB2—O1^i	2.369 (7)	O1—O2^lxi	3.364 (16)
PB2—O1^ii	2.379 (7)	O1—O2^lxii	3.269 (10)
PB2—O1^li	4.114 (8)	O1—O2^lxiii	3.310 (10)
PB2—O1^lii	4.068 (17)	O1—O2^lxiv	3.406 (17)
PB2—O1^liii	3.991 (12)	O1—O2^lxv	3.154 (17)
PB2—O1^liv	4.126 (10)	O2—PB1^xlix	2.567 (4)
PB2—O1^lv	4.246 (15)	O2—PB2^li	2.888 (13)
PB2—O1^lvi	3.826 (18)	O2—PB2^liii	2.659 (13)
PB2—O1^lvii	3.949 (14)	O2—PB2^liv	2.620 (19)
PB2—O1^lviii	4.240 (14)	O2—PB2^lvi	2.933 (18)
PB2—O1^lix	3.996 (12)	O2—PB2^lvii	2.902 (14)
PB2—O2^xiii	2.940 (9)	O2—PB2^lix	2.674 (13)
PB2—O2^xvii	2.750 (9)	O2—PB2^lxvi	2.981 (19)
PB2—O2^xviii	2.849 (4)	O2—PB2^lxi	2.572 (19)
PB2—O2^xxi	2.845 (4)	O2—PB2^lxii	2.707 (13)
PB2—O2^xxv	2.941 (9)	O2—PB2^lxiii	2.840 (13)
PB2—O2^xxix	2.751 (9)	O2—PB2^lxiv	2.722 (13)
PB2—O2^li	2.888 (13)	O2—PB2^lxviii	2.854 (14)
PB2—O2^liii	2.659 (13)	O2—PB2^xlix	2.940 (9)
PB2—O2^liv	2.674 (13)	O2—PB2^lxx	2.849 (4)
PB2—O2^lv	2.902 (14)	O2—PB2^lxxiii	2.750 (9)
PB2—O2^lviii	2.933 (18)	O2—PB2^lxxvi	2.845 (4)
PB2—O2^lix	2.620 (19)	O2—PB2^lxxix	2.941 (9)
PB2—O2^lx	2.981 (19)	O2—PB2^lxxxii	2.751 (9)
PB2—O2^lxi	2.572 (19)	O2—P^102	4.297 (8)
PB2—O2^lxii	2.840 (13)	O2—P	1.537 (4)
PB2—O2^lxiii	2.707 (13)	O2—P^103	4.265 (8)
PB2—O2^lxiv	2.722 (13)	O2—P^lxxxiv	3.635 (6)
PB2—O2^lxv	2.854 (14)	O2—P^li	4.327 (9)
P—PB1^xlviii	3.445 (2)	O2—P^liii	4.296 (9)
P—PB1^xlix	3.445 (2)	O2—O1	2.580 (12)
P—PB1^l	3.445 (2)	O2—O1^i	2.453 (7)
P—PB2	3.885 (8)	O2—O1^ii	2.455 (7)
P—PB2^i	3.885 (8)	O2—O1^li	3.310 (10)
P—PB2^ii	3.885 (8)	O2—O1^liii	3.269 (10)
P—PB2^iii	3.885 (8)	O2—O1^liv	3.406 (17)
P—PB2^iv	3.885 (8)	O2—O1^lvi	3.154 (17)
P—PB2^v	3.885 (8)	O2—O1^lvii	3.195 (16)
P—PB2^li	3.3189 (19)	O2—O1^lix	3.364 (16)
P—PB2^lii	3.467 (13)	O2—O2^i	2.508 (6)
P—PB2^liii	3.164 (13)	O2—O2^lxxxvii	2.934 (6)
P—PB2^liv	3.164 (13)	O2—O2^xc	2.934 (6)
P—PB2^lv	3.3189 (19)	O2—O2^ii	2.508 (6)
P—PB2^lvi	3.467 (13)	O2—O2^xcii	2.959 (13)
P—PB2^lvii	3.467 (13)	O2—O2^iii	2.483 (13)
P—PB2^lviii	3.164 (13)	O2—O2^iv	0.05 (2)
P—PB2^lix	3.3189 (19)	O2—O2^v	2.532 (13)
P—PB2^lxvi	3.467 (13)	O2—O2^xcv	2.909 (13)
P—PB2^lx	3.3189 (19)	O2—O2^104	4.350 (15)
P—PB2^lxi	3.164 (13)	O2—O2^lxxxiv	4.041 (7)
P—PB2^lxii	3.164 (13)	O2—O2^105	4.288 (15)
P—PB2^lxvii	3.467 (13)	O2—O2^xcvii	3.169 (6)
P—PB2^lxiii	3.3189 (19)	O2—O2^xcviii	3.169 (6)
P—PB2^lxiv	3.3189 (19)	O2—O2^xcix	3.189 (11)
P—PB2^lxv	3.164 (13)	O2—O2^106	4.319 (5)
P—PB2^lxviii	3.467 (13)	O2—O2^100	4.041 (7)
P—PB2^xlviii	4.089 (11)	O2—O2^107	4.319 (5)
P—PB2^xlix	4.328 (11)	O2—O2^101	3.150 (11)
P—PB2^l	4.210 (5)	O2—O2^liv	4.214 (6)
P—PB2^lxix	4.328 (11)	O2—O2^lix	4.214 (6)
P—PB2^lxx	4.210 (5)	O2—O2^lxi	4.197 (10)
P—PB2^lxxi	4.089 (11)	O2—O2^lxiv	4.231 (10)
PB2^i—PB2—PB2^ii	60.0000 (2)	O1^ii—P—O2	106.8 (4)
PB2^i—PB2—PB2^iii	90.0000 (11)	O1^ii—P—O2^i	106.7 (4)
PB2^i—PB2—PB2^iv	30.0000 (4)	O1^ii—P—O2^ii	115.1 (7)
PB2^i—PB2—PB2^v	30.0000 (1)	O1^ii—P—O2^iii	115.1 (7)
PB2^ii—PB2—PB2^iii	30.0000 (5)	O1^ii—P—O2^iv	106.7 (4)
PB2^ii—PB2—PB2^iv	90.0000 (11)	O1^ii—P—O2^v	106.8 (4)
PB2^ii—PB2—PB2^v	30.0000 (1)	O2—P—O2^i	109.3 (2)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	109.3 (2)
PB2^iii—PB2—PB2^v	60.0	O2—P—O2^iii	107.7 (8)
PB2^iv—PB2—PB2^v	60.0	O2—P—O2^iv	1.8 (8)
O1—P—O1^i	9.6 (12)	O2—P—O2^v	110.9 (8)
O1—P—O1^ii	9.6 (12)	O2^i—P—O2^ii	109.3 (2)
O1—P—O2	115.1 (7)	O2^i—P—O2^iii	110.9 (8)
O1—P—O2^i	106.8 (4)	O2^i—P—O2^iv	107.7 (8)
O1—P—O2^ii	106.7 (4)	O2^i—P—O2^v	1.8 (8)
O1—P—O2^iii	106.8 (4)	O2^ii—P—O2^iii	1.8 (8)
O1—P—O2^iv	115.1 (7)	O2^ii—P—O2^iv	110.9 (8)
O1—P—O2^v	106.7 (4)	O2^ii—P—O2^v	107.7 (8)
O1^i—P—O1^ii	9.6 (12)	O2^iii—P—O2^iv	109.3 (2)
O1^i—P—O2	106.7 (4)	O2^iii—P—O2^v	109.3 (2)
O1^i—P—O2^i	115.1 (7)	O2^iv—P—O2^v	109.3 (2)
O1^i—P—O2^ii	106.8 (4)	P—O1—O1^i	85.2 (6)
O1^i—P—O2^iii	106.7 (4)	P—O1—O1^ii	85.2 (6)
O1^i—P—O2^iv	106.8 (4)	O1^i—O1—O1^ii	60.0
O1^i—P—O2^v	115.1 (7)	P—O2—O2^iv	89.1 (4)

Symmetry codes: (i) −y, x−y, z; (ii) y−x, −x, z; (iii) y−x, y, z; (iv) −y, −x, z; (v) x, x−y, z; (vi) −x, −y, −z; (vii) y, y−x, −z; (viii) x−y, x, −z; (ix) x−y, −y, −z; (x) y, x, −z; (xi) −x, y−x, −z; (xii) x−2/3, y−1/3, z−1/3; (xiii) x+1/3, y−1/3, z−1/3; (xiv) x+1/3, y+2/3, z−1/3; (xv) −y−2/3, x−y−1/3, z−1/3; (xvi) −y+1/3, x−y−1/3, z−1/3; (xvii) −y+1/3, x−y+2/3, z−1/3; (xviii) y−x−2/3, −x−1/3, z−1/3; (xix) y−x+1/3, −x−1/3, z−1/3; (xx) y−x+1/3, −x+2/3, z−1/3; (xxi) y−x−2/3, y−1/3, z−1/3; (xxii) y−x+1/3, y−1/3, z−1/3; (xxiii) y−x+1/3, y+2/3, z−1/3; (xxiv) −y−2/3, −x−1/3, z−1/3; (xxv) −y+1/3, −x−1/3, z−1/3; (xxvi) −y+1/3, −x+2/3, z−1/3; (xxvii) x−2/3, x−y−1/3, z−1/3; (xxviii) x+1/3, x−y−1/3, z−1/3; (xxix) x+1/3, x−y+2/3, z−1/3; (xxx) −x−2/3, −y−1/3, −z+2/3; (xxxi) −x−2/3, −y+2/3, −z+2/3; (xxxii) −x+1/3, −y+2/3, −z+2/3; (xxxiii) y−2/3, y−x−1/3, −z+2/3; (xxxiv) y−2/3, y−x+2/3, −z+2/3; (xxxv) y+1/3, y−x+2/3, −z+2/3; (xxxvi) x−y−2/3, x−1/3, −z+2/3; (xxxvii) x−y−2/3, x+2/3, −z+2/3; (xxxviii) x−y+1/3, x+2/3, −z+2/3; (xxxix) x−y−2/3, −y−1/3, −z+2/3; (xl) x−y−2/3, −y+2/3, −z+2/3; (xli) x−y+1/3, −y+2/3, −z+2/3; (xlii) y−2/3, x−1/3, −z+2/3; (xliii) y−2/3, x+2/3, −z+2/3; (xliv) y+1/3, x+2/3, −z+2/3; (xlv) −x−2/3, y−x−1/3, −z+2/3; (xlvi) −x−2/3, y−x+2/3, −z+2/3; (xlvii) −x+1/3, y−x+2/3, −z+2/3; (xlviii) x−1/3, y−2/3, z+1/3; (xlix) x−1/3, y+1/3, z+1/3; (l) x+2/3, y+1/3, z+1/3; (li) −x−1/3, −y−2/3, −z+1/3; (lii) −x+2/3, −y−2/3, −z+1/3; (liii) −x+2/3, −y+1/3, −z+1/3; (liv) y−1/3, y−x−2/3, −z+1/3; (lv) y+2/3, y−x−2/3, −z+1/3; (lvi) y+2/3, y−x+1/3, −z+1/3; (lvii) x−y−1/3, x−2/3, −z+1/3; (lviii) x−y+2/3, x−2/3, −z+1/3; (lix) x−y+2/3, x+1/3, −z+1/3; (lx) x−y+2/3, −y−2/3, −z+1/3; (lxi) x−y+2/3, −y+1/3, −z+1/3; (lxii) y−1/3, x−2/3, −z+1/3; (lxiii) y+2/3, x+1/3, −z+1/3; (lxiv) −x−1/3, y−x−2/3, −z+1/3; (lxv) −x+2/3, y−x−2/3, −z+1/3; (lxvi) x−y−1/3, −y−2/3, −z+1/3; (lxvii) y+2/3, x−2/3, −z+1/3; (lxviii) −x+2/3, y−x+1/3, −z+1/3; (lxix) −y−1/3, x−y−2/3, z+1/3; (lxx) −y−1/3, x−y+1/3, z+1/3; (lxxi) −y+2/3, x−y+1/3, z+1/3; (lxxii) y−x−1/3, −x−2/3, z+1/3; (lxxiii) y−x−1/3, −x+1/3, z+1/3; (lxxiv) y−x+2/3, −x+1/3, z+1/3; (lxxv) y−x−1/3, y−2/3, z+1/3; (lxxvi) y−x−1/3, y+1/3, z+1/3; (lxxvii) y−x+2/3, y+1/3, z+1/3; (lxxviii) −y−1/3, −x−2/3, z+1/3; (lxxix) −y−1/3, −x+1/3, z+1/3; (lxxx) −y+2/3, −x+1/3, z+1/3; (lxxxi) x−1/3, x−y−2/3, z+1/3; (lxxxii) x−1/3, x−y+1/3, z+1/3; (lxxxiii) x+2/3, x−y+1/3, z+1/3; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) −y, x−y+1, z; (lxxxviii) −y+1, x−y+1, z; (lxxxix) y−x−1, −x−1, z; (xc) y−x−1, −x, z; (xci) y−x−1, y−1, z; (xcii) y−x−1, y, z; (xciii) −y, −x−1, z; (xciv) −y+1, −x, z; (xcv) x, x−y+1, z; (xcvi) x+1, x−y+1, z; (xcvii) y, y−x, −z+1; (xcviii) x−y, x, −z+1; (xcix) x−y, −y, −z+1; (100) y, x, −z+1; (101) −x, y−x, −z+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x−1, −y, −z+1; (105) −x, −y+1, −z+1; (106) y−1, x, −z+1; (107) y, x+1, −z+1.

(S4P29_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8982 (6) Å	T = 298 K
c = 2.8314 (10) Å	Particle morphology: Pressure cell anvil material
V = 20.60 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.042	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 80.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 7.51 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 131.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 275.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	37 parameters
Rexp = 0.026	9 restraints
R(F^2) = 0.20098	(Δ/σ)max = 0.07
χ^2 = 1.769	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.85806 2: -0.416774 3: 0.618934 4: -7.414880E-02 5: 0.229918 6: -8.061570E-02 7: 0.156447 8: -5.782420E-02 9: 8.559980E-0210: -3.797140E-0211: 4.114650E-0212: 5.205830E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92661 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.214 (4)	P—PB2	4.210 (5)
PB1—PB2^i	4.214 (4)	P—PB2	4.089 (11)
PB1—PB2^ii	4.214 (4)	P—PB2	4.328 (11)
PB1—PB2^iii	4.214 (4)	P—PB2	4.089 (11)
PB1—PB2^iv	4.214 (4)	P—PB2	4.210 (5)
PB1—PB2^v	4.214 (4)	P—PB2	4.328 (11)
PB1—PB2	4.214 (4)	P—PB2	4.210 (5)
PB1—PB2	4.214 (4)	P—PB2	4.328 (11)
PB1—PB2	4.214 (4)	P—PB2	4.089 (11)
PB1—PB2	4.214 (4)	P—PB2	4.328 (11)
PB1—PB2	4.214 (4)	P—PB2	4.089 (11)
PB1—PB2	4.214 (4)	P—PB2	4.210 (5)
PB1—PB2	3.999 (2)	P—P	3.850 (11)
PB1—PB2	3.871 (10)	P—P	4.226 (8)
PB1—PB2	4.122 (11)	P—P	4.226 (8)
PB1—PB2	4.122 (11)	P—P	4.226 (8)
PB1—PB2	3.999 (2)	P—O1	1.520 (6)
PB1—PB2	3.871 (10)	P—O1^i	1.520 (6)
PB1—PB2	3.871 (10)	P—O1^ii	1.520 (6)
PB1—PB2	4.122 (11)	P—O1	3.475 (10)
PB1—PB2	3.999 (2)	P—O1	3.271 (17)
PB1—PB2	3.871 (10)	P—O1	3.475 (10)
PB1—PB2	3.999 (2)	P—O1	3.475 (10)
PB1—PB2	4.122 (11)	P—O1	3.475 (10)
PB1—PB2	4.122 (11)	P—O1	3.271 (17)
PB1—PB2	3.871 (10)	P—O1	3.271 (17)
PB1—PB2	3.999 (2)	P—O1	3.475 (10)
PB1—PB2	3.999 (2)	P—O1	3.475 (10)
PB1—PB2	4.122 (11)	P—O2^vi	4.265 (8)
PB1—PB2	3.871 (10)	P—O2	1.537 (4)
PB1—PB2	4.122 (11)	P—O2^vii	4.297 (8)
PB1—PB2	3.871 (10)	P—O2^i	1.537 (4)
PB1—PB2	3.999 (2)	P—O2^viii	4.297 (8)
PB1—PB2	3.871 (10)	P—O2^ix	4.265 (8)
PB1—PB2	3.999 (2)	P—O2^x	4.297 (8)
PB1—PB2	4.122 (11)	P—O2^xi	4.265 (8)
PB1—PB2	3.999 (2)	P—O2^ii	1.537 (4)
PB1—PB2	4.122 (11)	P—O2^xii	4.265 (8)
PB1—PB2	3.871 (10)	P—O2^xiii	4.297 (8)
PB1—PB2	4.122 (11)	P—O2^iii	1.537 (4)
PB1—PB2	3.999 (2)	P—O2^xiv	4.297 (8)
PB1—PB2	3.871 (10)	P—O2^iv	1.537 (4)
PB1—PB2	3.999 (2)	P—O2^xv	4.265 (8)
PB1—PB2	3.871 (10)	P—O2^v	1.537 (4)
PB1—PB2	4.122 (11)	P—O2^xvi	4.265 (8)
PB1—PB2	3.871 (10)	P—O2^xvii	4.297 (8)
PB1—PB2	4.122 (11)	P—O2	3.635 (6)
PB1—PB2	3.999 (2)	P—O2	3.635 (6)
PB1—P	3.445 (2)	P—O2	3.635 (6)
PB1—P	3.445 (2)	P—O2	3.635 (6)
PB1—P	3.445 (2)	P—O2	3.635 (6)
PB1—P	3.445 (2)	P—O2	3.635 (6)
PB1—P	3.445 (2)	P—O2	4.327 (9)
PB1—P	3.445 (2)	P—O2	4.296 (9)
PB1—O1	3.073 (9)	P—O2	4.296 (9)
PB1—O1	3.290 (18)	P—O2	4.327 (9)
PB1—O1	3.073 (9)	P—O2	4.296 (9)
PB1—O1	3.073 (9)	P—O2	4.327 (9)
PB1—O1	3.073 (9)	P—O2	4.327 (9)
PB1—O1	3.290 (18)	P—O2	4.296 (9)
PB1—O1	3.290 (18)	P—O2	4.296 (9)
PB1—O1	3.073 (9)	P—O2	4.327 (9)
PB1—O1	3.073 (9)	P—O2	4.327 (9)
PB1—O1	3.073 (9)	P—O2	4.296 (9)
PB1—O1	3.290 (18)	O1—PB1	3.073 (9)
PB1—O1	3.073 (9)	O1—PB1	3.290 (18)
PB1—O1	3.290 (18)	O1—PB1	3.073 (9)
PB1—O1	3.073 (9)	O1—PB2	2.389 (7)
PB1—O1	3.073 (9)	O1—PB2^i	2.379 (7)
PB1—O1	3.073 (9)	O1—PB2^ii	2.369 (7)
PB1—O1	3.073 (9)	O1—PB2^iii	2.379 (7)
PB1—O1	3.290 (18)	O1—PB2^iv	2.389 (7)
PB1—O2	2.567 (4)	O1—PB2^v	2.369 (7)
PB1—O2	2.567 (4)	O1—PB2	4.114 (8)
PB1—O2	2.567 (4)	O1—PB2	4.068 (17)
PB1—O2	2.567 (4)	O1—PB2	3.991 (12)
PB1—O2	2.567 (4)	O1—PB2	3.996 (12)
PB1—O2	2.567 (4)	O1—PB2	3.949 (14)
PB1—O2	2.567 (4)	O1—PB2	4.240 (14)
PB1—O2	2.567 (4)	O1—PB2	4.246 (15)
PB1—O2	2.567 (4)	O1—PB2	3.826 (18)
PB1—O2	2.567 (4)	O1—PB2	4.126 (10)
PB1—O2	2.567 (4)	O1—PB2	4.240 (14)
PB1—O2	2.567 (4)	O1—PB2	3.949 (14)
PB2—PB1	4.214 (4)	O1—PB2	3.996 (12)
PB2—PB1	4.122 (11)	O1—PB2	3.991 (12)
PB2—PB1	3.871 (10)	O1—PB2	4.068 (17)
PB2—PB1	3.999 (2)	O1—PB2	4.114 (8)
PB2—PB2^i	0.32 (3)	O1—PB2	4.126 (10)
PB2—PB2^ii	0.32 (3)	O1—PB2	3.826 (18)
PB2—PB2^iii	0.184 (15)	O1—PB2	4.246 (15)
PB2—PB2^iv	0.184 (15)	O1—P	1.520 (6)
PB2—PB2^v	0.37 (3)	O1—P	3.475 (10)
PB2—PB2	3.88 (3)	O1—P	3.271 (17)
PB2—PB2	3.32 (2)	O1—P	3.475 (10)
PB2—PB2	3.611 (5)	O1—O1^i	0.25 (3)
PB2—PB2	3.597 (4)	O1—O1^ii	0.25 (3)
PB2—PB2	3.455 (12)	O1—O1	3.30 (2)
PB2—PB2	3.734 (13)	O1—O1	2.86 (4)
PB2—PB2	3.734 (13)	O1—O1	3.30 (2)
PB2—PB2	3.597 (4)	O1—O1	3.294 (18)
PB2—PB2	3.455 (12)	O1—O1	3.077 (9)
PB2—PB2	3.88 (2)	O1—O1	3.077 (9)
PB2—PB2	3.465 (10)	O1—O1	3.077 (9)
PB2—PB2	3.465 (10)	O1—O1	3.077 (9)
PB2—PB2	3.743 (14)	O1—O1	3.294 (18)
PB2—PB2	3.32 (2)	O1—O2	2.580 (12)
PB2—PB2	3.743 (14)	O1—O2^i	2.455 (7)
PB2—PB2	3.593 (4)	O1—O2^ii	2.453 (7)
PB2—PB2	3.593 (4)	O1—O2^iii	2.455 (7)
PB2—PB2	3.593 (4)	O1—O2^iv	2.580 (12)
PB2—P	3.885 (8)	O1—O2^v	2.453 (7)
PB2—P	4.210 (5)	O1—O2	3.310 (10)
PB2—P	4.328 (11)	O1—O2	3.269 (10)
PB2—P	4.089 (11)	O1—O2	3.364 (16)
PB2—P	3.3189 (19)	O1—O2	3.195 (16)
PB2—P	3.467 (13)	O1—O2	3.154 (17)
PB2—P	3.164 (13)	O1—O2	3.406 (17)
PB2—O1	2.389 (7)	O1—O2	3.195 (16)
PB2—O1^i	2.369 (7)	O1—O2	3.364 (16)
PB2—O1^ii	2.379 (7)	O1—O2	3.269 (10)
PB2—O1	4.114 (8)	O1—O2	3.310 (10)
PB2—O1	4.068 (17)	O1—O2	3.406 (17)
PB2—O1	3.991 (12)	O1—O2	3.154 (17)
PB2—O1	4.126 (10)	O2—PB1	2.567 (4)
PB2—O1	4.246 (15)	O2—PB2	2.888 (13)
PB2—O1	3.826 (18)	O2—PB2	2.659 (13)
PB2—O1	3.949 (14)	O2—PB2	2.620 (19)
PB2—O1	4.240 (14)	O2—PB2	2.933 (18)
PB2—O1	3.996 (12)	O2—PB2	2.902 (14)
PB2—O2	2.940 (9)	O2—PB2	2.674 (13)
PB2—O2	2.750 (9)	O2—PB2	2.981 (19)
PB2—O2	2.849 (4)	O2—PB2	2.572 (19)
PB2—O2	2.845 (4)	O2—PB2	2.707 (13)
PB2—O2	2.941 (9)	O2—PB2	2.840 (13)
PB2—O2	2.751 (9)	O2—PB2	2.722 (13)
PB2—O2	2.888 (13)	O2—PB2	2.854 (14)
PB2—O2	2.659 (13)	O2—PB2	2.940 (9)
PB2—O2	2.674 (13)	O2—PB2	2.849 (4)
PB2—O2	2.902 (14)	O2—PB2	2.750 (9)
PB2—O2	2.933 (18)	O2—PB2	2.845 (4)
PB2—O2	2.620 (19)	O2—PB2	2.941 (9)
PB2—O2	2.981 (19)	O2—PB2	2.751 (9)
PB2—O2	2.572 (19)	O2—P^xviii	4.297 (8)
PB2—O2	2.840 (13)	O2—P	1.537 (4)
PB2—O2	2.707 (13)	O2—P^xix	4.265 (8)
PB2—O2	2.722 (13)	O2—P	3.635 (6)
PB2—O2	2.854 (14)	O2—P	4.327 (9)
P—PB1	3.445 (2)	O2—P	4.296 (9)
P—PB1	3.445 (2)	O2—O1	2.580 (12)
P—PB1	3.445 (2)	O2—O1^i	2.453 (7)
P—PB2	3.885 (8)	O2—O1^ii	2.455 (7)
P—PB2^i	3.885 (8)	O2—O1	3.310 (10)
P—PB2^ii	3.885 (8)	O2—O1	3.269 (10)
P—PB2^iii	3.885 (8)	O2—O1	3.406 (17)
P—PB2^iv	3.885 (8)	O2—O1	3.154 (17)
P—PB2^v	3.885 (8)	O2—O1	3.195 (16)
P—PB2	3.3189 (19)	O2—O1	3.364 (16)
P—PB2	3.467 (13)	O2—O2^i	2.508 (6)
P—PB2	3.164 (13)	O2—O2^viii	2.934 (6)
P—PB2	3.164 (13)	O2—O2^xi	2.934 (6)
P—PB2	3.3189 (19)	O2—O2^ii	2.508 (6)
P—PB2	3.467 (13)	O2—O2^xiii	2.959 (13)
P—PB2	3.467 (13)	O2—O2^iii	2.483 (13)
P—PB2	3.164 (13)	O2—O2^iv	0.05 (2)
P—PB2	3.3189 (19)	O2—O2^v	2.532 (13)
P—PB2	3.467 (13)	O2—O2^xvi	2.909 (13)
P—PB2	3.3189 (19)	O2—O2	4.350 (15)
P—PB2	3.164 (13)	O2—O2	4.041 (7)
P—PB2	3.164 (13)	O2—O2	4.288 (15)
P—PB2	3.467 (13)	O2—O2	3.169 (6)
P—PB2	3.3189 (19)	O2—O2	3.169 (6)
P—PB2	3.3189 (19)	O2—O2	3.189 (11)
P—PB2	3.164 (13)	O2—O2	4.319 (5)
P—PB2	3.467 (13)	O2—O2	4.041 (7)
P—PB2	4.089 (11)	O2—O2	4.319 (5)
P—PB2	4.328 (11)	O2—O2	3.150 (11)
P—PB2	4.210 (5)	O2—O2	4.214 (6)
P—PB2	4.328 (11)	O2—O2	4.214 (6)
P—PB2	4.210 (5)	O2—O2	4.197 (10)
P—PB2	4.089 (11)	O2—O2	4.231 (10)
PB2^i—PB2—PB2^ii	60.0000 (2)	O1^ii—P—O2	106.8 (4)
PB2^i—PB2—PB2^iii	90.0000 (11)	O1^ii—P—O2^i	106.7 (4)
PB2^i—PB2—PB2^iv	30.0000 (4)	O1^ii—P—O2^ii	115.1 (7)
PB2^i—PB2—PB2^v	30.0000 (1)	O1^ii—P—O2^iii	115.1 (7)
PB2^ii—PB2—PB2^iii	30.0000 (5)	O1^ii—P—O2^iv	106.7 (4)
PB2^ii—PB2—PB2^iv	90.0000 (11)	O1^ii—P—O2^v	106.8 (4)
PB2^ii—PB2—PB2^v	30.0000 (1)	O2—P—O2^i	109.3 (2)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	109.3 (2)
PB2^iii—PB2—PB2^v	60.0	O2—P—O2^iii	107.7 (8)
PB2^iv—PB2—PB2^v	60.0	O2—P—O2^iv	1.8 (8)
O1—P—O1^i	9.6 (12)	O2—P—O2^v	110.9 (8)
O1—P—O1^ii	9.6 (12)	O2^i—P—O2^ii	109.3 (2)
O1—P—O2	115.1 (7)	O2^i—P—O2^iii	110.9 (8)
O1—P—O2^i	106.8 (4)	O2^i—P—O2^iv	107.7 (8)
O1—P—O2^ii	106.7 (4)	O2^i—P—O2^v	1.8 (8)
O1—P—O2^iii	106.8 (4)	O2^ii—P—O2^iii	1.8 (8)
O1—P—O2^iv	115.1 (7)	O2^ii—P—O2^iv	110.9 (8)
O1—P—O2^v	106.7 (4)	O2^ii—P—O2^v	107.7 (8)
O1^i—P—O1^ii	9.6 (12)	O2^iii—P—O2^iv	109.3 (2)
O1^i—P—O2	106.7 (4)	O2^iii—P—O2^v	109.3 (2)
O1^i—P—O2^i	115.1 (7)	O2^iv—P—O2^v	109.3 (2)
O1^i—P—O2^ii	106.8 (4)	P—O1—O1^i	85.2 (6)
O1^i—P—O2^iii	106.7 (4)	P—O1—O1^ii	85.2 (6)
O1^i—P—O2^iv	106.8 (4)	O1^i—O1—O1^ii	60.0
O1^i—P—O2^v	115.1 (7)	P—O2—O2^iv	89.1 (4)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) x, y, −z; (iv) y−x, −x, z; (v) −y, x−y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) y−x, −x+1, −z; (ix) y−x+1, −x+1, −z; (x) −y−1, x−y−1, z; (xi) −y−1, x−y, z; (xii) x−1, y−1, −z; (xiii) x−1, y, −z; (xiv) y−x, −x−1, z; (xv) y−x+1, −x, z; (xvi) −y, x−y+1, −z; (xvii) −y+1, x−y+1, −z; (xviii) x−1, y, z; (xix) x, y+1, z.

(S4P29_phase_3)

Crystal data

Ni	anvil material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5442 (8) Å	Particle morphology: Component of pressure cell, not sample
V = 44.52 (3) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.042	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 80.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 7.51 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 131.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 275.9 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.035	37 parameters
Rexp = 0.026	9 restraints
R(F^2) = 0.20098	(Δ/σ)max = 0.07
χ^2 = 1.769	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.85806 2: -0.416774 3: 0.618934 4: -7.414880E-02 5: 0.229918 6: -8.061570E-02 7: 0.156447 8: -5.782420E-02 9: 8.559980E-0210: -3.797140E-0211: 4.114650E-0212: 5.205830E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92661 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.214 (4)	P—PB2^lxxii	4.210 (5)
PB1—PB2^i	4.214 (4)	P—PB2^lxxiii	4.089 (11)
PB1—PB2^ii	4.214 (4)	P—PB2^lxxiv	4.328 (11)
PB1—PB2^iii	4.214 (4)	P—PB2^lxxv	4.089 (11)
PB1—PB2^iv	4.214 (4)	P—PB2^lxxvi	4.210 (5)
PB1—PB2^v	4.214 (4)	P—PB2^lxxvii	4.328 (11)
PB1—PB2^vi	4.214 (4)	P—PB2^lxxviii	4.210 (5)
PB1—PB2^vii	4.214 (4)	P—PB2^lxxix	4.328 (11)
PB1—PB2^viii	4.214 (4)	P—PB2^lxxx	4.089 (11)
PB1—PB2^ix	4.214 (4)	P—PB2^lxxxi	4.328 (11)
PB1—PB2^x	4.214 (4)	P—PB2^lxxxii	4.089 (11)
PB1—PB2^xi	4.214 (4)	P—PB2^lxxxiii	4.210 (5)
PB1—PB2^xii	3.999 (2)	P—P^lxxxiv	3.850 (11)
PB1—PB2^xiii	3.871 (10)	P—P^li	4.226 (8)
PB1—PB2^xiv	4.122 (11)	P—P^lii	4.226 (8)
PB1—PB2^xv	4.122 (11)	P—P^liii	4.226 (8)
PB1—PB2^xvi	3.999 (2)	P—O1	1.520 (6)
PB1—PB2^xvii	3.871 (10)	P—O1^i	1.520 (6)
PB1—PB2^xviii	3.871 (10)	P—O1^ii	1.520 (6)
PB1—PB2^xix	4.122 (11)	P—O1^li	3.475 (10)
PB1—PB2^xx	3.999 (2)	P—O1^lii	3.271 (17)
PB1—PB2^xxi	3.871 (10)	P—O1^liii	3.475 (10)
PB1—PB2^xxii	3.999 (2)	P—O1^liv	3.475 (10)
PB1—PB2^xxiii	4.122 (11)	P—O1^lv	3.475 (10)
PB1—PB2^xxiv	4.122 (11)	P—O1^lvi	3.271 (17)
PB1—PB2^xxv	3.871 (10)	P—O1^lvii	3.271 (17)
PB1—PB2^xxvi	3.999 (2)	P—O1^lviii	3.475 (10)
PB1—PB2^xxvii	3.999 (2)	P—O1^lix	3.475 (10)
PB1—PB2^xxviii	4.122 (11)	P—O2^lxxxv	4.265 (8)
PB1—PB2^xxix	3.871 (10)	P—O2	1.537 (4)
PB1—PB2^xxx	4.122 (11)	P—O2^lxxxvi	4.297 (8)
PB1—PB2^xxxi	3.871 (10)	P—O2^i	1.537 (4)
PB1—PB2^xxxii	3.999 (2)	P—O2^lxxxvii	4.297 (8)
PB1—PB2^xxxiii	3.871 (10)	P—O2^lxxxviii	4.265 (8)
PB1—PB2^xxxiv	3.999 (2)	P—O2^lxxxix	4.297 (8)
PB1—PB2^xxxv	4.122 (11)	P—O2^xc	4.265 (8)
PB1—PB2^xxxvi	3.999 (2)	P—O2^ii	1.537 (4)
PB1—PB2^xxxvii	4.122 (11)	P—O2^xci	4.265 (8)
PB1—PB2^xxxviii	3.871 (10)	P—O2^xcii	4.297 (8)
PB1—PB2^xxxix	4.122 (11)	P—O2^iii	1.537 (4)
PB1—PB2^xl	3.999 (2)	P—O2^xciii	4.297 (8)
PB1—PB2^xli	3.871 (10)	P—O2^iv	1.537 (4)
PB1—PB2^xlii	3.999 (2)	P—O2^xciv	4.265 (8)
PB1—PB2^xliii	3.871 (10)	P—O2^v	1.537 (4)
PB1—PB2^xliv	4.122 (11)	P—O2^xcv	4.265 (8)
PB1—PB2^xlv	3.871 (10)	P—O2^xcvi	4.297 (8)
PB1—PB2^xlvi	4.122 (11)	P—O2^lxxxiv	3.635 (6)
PB1—PB2^xlvii	3.999 (2)	P—O2^xcvii	3.635 (6)
PB1—P^xii	3.445 (2)	P—O2^xcviii	3.635 (6)
PB1—P^xiii	3.445 (2)	P—O2^xcix	3.635 (6)
PB1—P^xiv	3.445 (2)	P—O2^100	3.635 (6)
PB1—P^xxx	3.445 (2)	P—O2^101	3.635 (6)
PB1—P^xxxi	3.445 (2)	P—O2^li	4.327 (9)
PB1—P^xxxii	3.445 (2)	P—O2^liii	4.296 (9)
PB1—O1^xii	3.073 (9)	P—O2^liv	4.296 (9)
PB1—O1^xiii	3.290 (18)	P—O2^lv	4.327 (9)
PB1—O1^xiv	3.073 (9)	P—O2^lviii	4.296 (9)
PB1—O1^xv	3.073 (9)	P—O2^lix	4.327 (9)
PB1—O1^xvi	3.073 (9)	P—O2^lx	4.327 (9)
PB1—O1^xvii	3.290 (18)	P—O2^lxi	4.296 (9)
PB1—O1^xviii	3.290 (18)	P—O2^lxii	4.296 (9)
PB1—O1^xix	3.073 (9)	P—O2^lxiii	4.327 (9)
PB1—O1^xx	3.073 (9)	P—O2^lxiv	4.327 (9)
PB1—O1^xxx	3.073 (9)	P—O2^lxv	4.296 (9)
PB1—O1^xxxi	3.290 (18)	O1—PB1^xlviii	3.073 (9)
PB1—O1^xxxii	3.073 (9)	O1—PB1^xlix	3.290 (18)
PB1—O1^xxxiii	3.290 (18)	O1—PB1^l	3.073 (9)
PB1—O1^xxxiv	3.073 (9)	O1—PB2	2.389 (7)
PB1—O1^xxxv	3.073 (9)	O1—PB2^i	2.379 (7)
PB1—O1^xxxvi	3.073 (9)	O1—PB2^ii	2.369 (7)
PB1—O1^xxxvii	3.073 (9)	O1—PB2^iii	2.379 (7)
PB1—O1^xxxviii	3.290 (18)	O1—PB2^iv	2.389 (7)
PB1—O2^xiii	2.567 (4)	O1—PB2^v	2.369 (7)
PB1—O2^xvii	2.567 (4)	O1—PB2^li	4.114 (8)
PB1—O2^xviii	2.567 (4)	O1—PB2^lii	4.068 (17)
PB1—O2^xxi	2.567 (4)	O1—PB2^liii	3.991 (12)
PB1—O2^xxv	2.567 (4)	O1—PB2^liv	3.996 (12)
PB1—O2^xxix	2.567 (4)	O1—PB2^lv	3.949 (14)
PB1—O2^xxxi	2.567 (4)	O1—PB2^lvi	4.240 (14)
PB1—O2^xxxiii	2.567 (4)	O1—PB2^lvii	4.246 (15)
PB1—O2^xxxviii	2.567 (4)	O1—PB2^lviii	3.826 (18)
PB1—O2^xli	2.567 (4)	O1—PB2^lix	4.126 (10)
PB1—O2^xliii	2.567 (4)	O1—PB2^lxvi	4.240 (14)
PB1—O2^xlv	2.567 (4)	O1—PB2^lx	3.949 (14)
PB2—PB1	4.214 (4)	O1—PB2^lxi	3.996 (12)
PB2—PB1^xlviii	4.122 (11)	O1—PB2^lxii	3.991 (12)
PB2—PB1^xlix	3.871 (10)	O1—PB2^lxvii	4.068 (17)
PB2—PB1^l	3.999 (2)	O1—PB2^lxiii	4.114 (8)
PB2—PB2^i	0.32 (3)	O1—PB2^lxiv	4.126 (10)
PB2—PB2^ii	0.32 (3)	O1—PB2^lxv	3.826 (18)
PB2—PB2^iii	0.184 (15)	O1—PB2^lxviii	4.246 (15)
PB2—PB2^iv	0.184 (15)	O1—P	1.520 (6)
PB2—PB2^v	0.37 (3)	O1—P^li	3.475 (10)
PB2—PB2^xxx	3.88 (3)	O1—P^lii	3.271 (17)
PB2—PB2^xxxi	3.32 (2)	O1—P^liii	3.475 (10)
PB2—PB2^xxxii	3.611 (5)	O1—O1^i	0.25 (3)
PB2—PB2^xxxiii	3.597 (4)	O1—O1^ii	0.25 (3)
PB2—PB2^xxxiv	3.455 (12)	O1—O1^li	3.30 (2)
PB2—PB2^xxxv	3.734 (13)	O1—O1^lii	2.86 (4)
PB2—PB2^xxxvi	3.734 (13)	O1—O1^liii	3.30 (2)
PB2—PB2^xxxvii	3.597 (4)	O1—O1^liv	3.294 (18)
PB2—PB2^xxxviii	3.455 (12)	O1—O1^lv	3.077 (9)
PB2—PB2^xxxix	3.88 (2)	O1—O1^lvi	3.077 (9)
PB2—PB2^xl	3.465 (10)	O1—O1^lvii	3.077 (9)
PB2—PB2^xli	3.465 (10)	O1—O1^lviii	3.077 (9)
PB2—PB2^xlii	3.743 (14)	O1—O1^lix	3.294 (18)
PB2—PB2^xliii	3.32 (2)	O1—O2	2.580 (12)
PB2—PB2^xliv	3.743 (14)	O1—O2^i	2.455 (7)
PB2—PB2^xlv	3.593 (4)	O1—O2^ii	2.453 (7)
PB2—PB2^xlvi	3.593 (4)	O1—O2^iii	2.455 (7)
PB2—PB2^xlvii	3.593 (4)	O1—O2^iv	2.580 (12)
PB2—P	3.885 (8)	O1—O2^v	2.453 (7)
PB2—P^xii	4.210 (5)	O1—O2^li	3.310 (10)
PB2—P^xiii	4.328 (11)	O1—O2^liii	3.269 (10)
PB2—P^xiv	4.089 (11)	O1—O2^liv	3.364 (16)
PB2—P^li	3.3189 (19)	O1—O2^lv	3.195 (16)
PB2—P^lii	3.467 (13)	O1—O2^lviii	3.154 (17)
PB2—P^liii	3.164 (13)	O1—O2^lix	3.406 (17)
PB2—O1	2.389 (7)	O1—O2^lx	3.195 (16)
PB2—O1^i	2.369 (7)	O1—O2^lxi	3.364 (16)
PB2—O1^ii	2.379 (7)	O1—O2^lxii	3.269 (10)
PB2—O1^li	4.114 (8)	O1—O2^lxiii	3.310 (10)
PB2—O1^lii	4.068 (17)	O1—O2^lxiv	3.406 (17)
PB2—O1^liii	3.991 (12)	O1—O2^lxv	3.154 (17)
PB2—O1^liv	4.126 (10)	O2—PB1^xlix	2.567 (4)
PB2—O1^lv	4.246 (15)	O2—PB2^li	2.888 (13)
PB2—O1^lvi	3.826 (18)	O2—PB2^liii	2.659 (13)
PB2—O1^lvii	3.949 (14)	O2—PB2^liv	2.620 (19)
PB2—O1^lviii	4.240 (14)	O2—PB2^lvi	2.933 (18)
PB2—O1^lix	3.996 (12)	O2—PB2^lvii	2.902 (14)
PB2—O2^xiii	2.940 (9)	O2—PB2^lix	2.674 (13)
PB2—O2^xvii	2.750 (9)	O2—PB2^lxvi	2.981 (19)
PB2—O2^xviii	2.849 (4)	O2—PB2^lxi	2.572 (19)
PB2—O2^xxi	2.845 (4)	O2—PB2^lxii	2.707 (13)
PB2—O2^xxv	2.941 (9)	O2—PB2^lxiii	2.840 (13)
PB2—O2^xxix	2.751 (9)	O2—PB2^lxiv	2.722 (13)
PB2—O2^li	2.888 (13)	O2—PB2^lxviii	2.854 (14)
PB2—O2^liii	2.659 (13)	O2—PB2^xlix	2.940 (9)
PB2—O2^liv	2.674 (13)	O2—PB2^lxx	2.849 (4)
PB2—O2^lv	2.902 (14)	O2—PB2^lxxiii	2.750 (9)
PB2—O2^lviii	2.933 (18)	O2—PB2^lxxvi	2.845 (4)
PB2—O2^lix	2.620 (19)	O2—PB2^lxxix	2.941 (9)
PB2—O2^lx	2.981 (19)	O2—PB2^lxxxii	2.751 (9)
PB2—O2^lxi	2.572 (19)	O2—P^102	4.297 (8)
PB2—O2^lxii	2.840 (13)	O2—P	1.537 (4)
PB2—O2^lxiii	2.707 (13)	O2—P^103	4.265 (8)
PB2—O2^lxiv	2.722 (13)	O2—P^lxxxiv	3.635 (6)
PB2—O2^lxv	2.854 (14)	O2—P^li	4.327 (9)
P—PB1^xlviii	3.445 (2)	O2—P^liii	4.296 (9)
P—PB1^xlix	3.445 (2)	O2—O1	2.580 (12)
P—PB1^l	3.445 (2)	O2—O1^i	2.453 (7)
P—PB2	3.885 (8)	O2—O1^ii	2.455 (7)
P—PB2^i	3.885 (8)	O2—O1^li	3.310 (10)
P—PB2^ii	3.885 (8)	O2—O1^liii	3.269 (10)
P—PB2^iii	3.885 (8)	O2—O1^liv	3.406 (17)
P—PB2^iv	3.885 (8)	O2—O1^lvi	3.154 (17)
P—PB2^v	3.885 (8)	O2—O1^lvii	3.195 (16)
P—PB2^li	3.3189 (19)	O2—O1^lix	3.364 (16)
P—PB2^lii	3.467 (13)	O2—O2^i	2.508 (6)
P—PB2^liii	3.164 (13)	O2—O2^lxxxvii	2.934 (6)
P—PB2^liv	3.164 (13)	O2—O2^xc	2.934 (6)
P—PB2^lv	3.3189 (19)	O2—O2^ii	2.508 (6)
P—PB2^lvi	3.467 (13)	O2—O2^xcii	2.959 (13)
P—PB2^lvii	3.467 (13)	O2—O2^iii	2.483 (13)
P—PB2^lviii	3.164 (13)	O2—O2^iv	0.05 (2)
P—PB2^lix	3.3189 (19)	O2—O2^v	2.532 (13)
P—PB2^lxvi	3.467 (13)	O2—O2^xcv	2.909 (13)
P—PB2^lx	3.3189 (19)	O2—O2^104	4.350 (15)
P—PB2^lxi	3.164 (13)	O2—O2^lxxxiv	4.041 (7)
P—PB2^lxii	3.164 (13)	O2—O2^105	4.288 (15)
P—PB2^lxvii	3.467 (13)	O2—O2^xcvii	3.169 (6)
P—PB2^lxiii	3.3189 (19)	O2—O2^xcviii	3.169 (6)
P—PB2^lxiv	3.3189 (19)	O2—O2^xcix	3.189 (11)
P—PB2^lxv	3.164 (13)	O2—O2^106	4.319 (5)
P—PB2^lxviii	3.467 (13)	O2—O2^100	4.041 (7)
P—PB2^xlviii	4.089 (11)	O2—O2^107	4.319 (5)
P—PB2^xlix	4.328 (11)	O2—O2^101	3.150 (11)
P—PB2^l	4.210 (5)	O2—O2^liv	4.214 (6)
P—PB2^lxix	4.328 (11)	O2—O2^lix	4.214 (6)
P—PB2^lxx	4.210 (5)	O2—O2^lxi	4.197 (10)
P—PB2^lxxi	4.089 (11)	O2—O2^lxiv	4.231 (10)
PB2^i—PB2—PB2^ii	60.0000 (2)	O1^ii—P—O2	106.8 (4)
PB2^i—PB2—PB2^iii	90.0000 (11)	O1^ii—P—O2^i	106.7 (4)
PB2^i—PB2—PB2^iv	30.0000 (4)	O1^ii—P—O2^ii	115.1 (7)
PB2^i—PB2—PB2^v	30.0000 (1)	O1^ii—P—O2^iii	115.1 (7)
PB2^ii—PB2—PB2^iii	30.0000 (5)	O1^ii—P—O2^iv	106.7 (4)
PB2^ii—PB2—PB2^iv	90.0000 (11)	O1^ii—P—O2^v	106.8 (4)
PB2^ii—PB2—PB2^v	30.0000 (1)	O2—P—O2^i	109.3 (2)
PB2^iii—PB2—PB2^iv	120.0	O2—P—O2^ii	109.3 (2)
PB2^iii—PB2—PB2^v	60.0	O2—P—O2^iii	107.7 (8)
PB2^iv—PB2—PB2^v	60.0	O2—P—O2^iv	1.8 (8)
O1—P—O1^i	9.6 (12)	O2—P—O2^v	110.9 (8)
O1—P—O1^ii	9.6 (12)	O2^i—P—O2^ii	109.3 (2)
O1—P—O2	115.1 (7)	O2^i—P—O2^iii	110.9 (8)
O1—P—O2^i	106.8 (4)	O2^i—P—O2^iv	107.7 (8)
O1—P—O2^ii	106.7 (4)	O2^i—P—O2^v	1.8 (8)
O1—P—O2^iii	106.8 (4)	O2^ii—P—O2^iii	1.8 (8)
O1—P—O2^iv	115.1 (7)	O2^ii—P—O2^iv	110.9 (8)
O1—P—O2^v	106.7 (4)	O2^ii—P—O2^v	107.7 (8)
O1^i—P—O1^ii	9.6 (12)	O2^iii—P—O2^iv	109.3 (2)
O1^i—P—O2	106.7 (4)	O2^iii—P—O2^v	109.3 (2)
O1^i—P—O2^i	115.1 (7)	O2^iv—P—O2^v	109.3 (2)
O1^i—P—O2^ii	106.8 (4)	P—O1—O1^i	85.2 (6)
O1^i—P—O2^iii	106.7 (4)	P—O1—O1^ii	85.2 (6)
O1^i—P—O2^iv	106.8 (4)	O1^i—O1—O1^ii	60.0
O1^i—P—O2^v	115.1 (7)	P—O2—O2^iv	89.1 (4)

Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) x, y, −z; (iv) −z, x, y; (v) y, −z, x; (vi) −x, −y, −z; (vii) −z, −x, −y; (viii) −y, −z, −x; (ix) −x, −y, z; (x) z, −x, −y; (xi) −y, z, −x; (xii) x−1, y−1/2, z−1/2; (xiii) x, y−1/2, z−1/2; (xiv) x, y+1/2, z−1/2; (xv) z−1, x−1/2, y−1/2; (xvi) z, x−1/2, y−1/2; (xvii) z, x+1/2, y−1/2; (xviii) y−1, z−1/2, x−1/2; (xix) y, z−1/2, x−1/2; (xx) y, z+1/2, x−1/2; (xxi) x−1, y−1/2, −z−1/2; (xxii) x, y−1/2, −z−1/2; (xxiii) x, y+1/2, −z−1/2; (xxiv) −z−1, x−1/2, y−1/2; (xxv) −z, x−1/2, y−1/2; (xxvi) −z, x+1/2, y−1/2; (xxvii) y−1, −z−1/2, x−1/2; (xxviii) y, −z−1/2, x−1/2; (xxix) y, −z+1/2, x−1/2; (xxx) −x−1/2, −y−1, −z+1/2; (xxxi) −x−1/2, −y, −z+1/2; (xxxii) −x+1/2, −y, −z+1/2; (xxxiii) −z−1/2, −x−1, −y+1/2; (xxxiv) −z−1/2, −x, −y+1/2; (xxxv) −z+1/2, −x, −y+1/2; (xxxvi) −y−1/2, −z−1, −x+1/2; (xxxvii) −y−1/2, −z, −x+1/2; (xxxviii) −y+1/2, −z, −x+1/2; (xxxix) −x−1/2, −y−1, z+1/2; (xl) −x−1/2, −y, z+1/2; (xli) −x+1/2, −y, z+1/2; (xlii) z−1/2, −x−1, −y+1/2; (xliii) z−1/2, −x, −y+1/2; (xliv) z+1/2, −x, −y+1/2; (xlv) −y−1/2, z−1, −x+1/2; (xlvi) −y−1/2, z, −x+1/2; (xlvii) −y+1/2, z, −x+1/2; (xlviii) x−1/2, y−1, z+1/2; (xlix) x−1/2, y, z+1/2; (l) x+1/2, y, z+1/2; (li) −x−1, −y−1/2, −z+1/2; (lii) −x, −y−1/2, −z+1/2; (liii) −x, −y+1/2, −z+1/2; (liv) −z−1, −x−1/2, −y+1/2; (lv) −z, −x−1/2, −y+1/2; (lvi) −z, −x+1/2, −y+1/2; (lvii) −y−1, −z−1/2, −x+1/2; (lviii) −y, −z−1/2, −x+1/2; (lix) −y, −z+1/2, −x+1/2; (lx) −x, −y−1/2, z+1/2; (lxi) −x, −y+1/2, z+1/2; (lxii) z−1, −x−1/2, −y+1/2; (lxiii) z, −x+1/2, −y+1/2; (lxiv) −y−1, z−1/2, −x+1/2; (lxv) −y, z−1/2, −x+1/2; (lxvi) −x−1, −y−1/2, z+1/2; (lxvii) z, −x−1/2, −y+1/2; (lxviii) −y, z+1/2, −x+1/2; (lxix) z−1/2, x−1, y+1/2; (lxx) z−1/2, x, y+1/2; (lxxi) z+1/2, x, y+1/2; (lxxii) y−1/2, z−1, x+1/2; (lxxiii) y−1/2, z, x+1/2; (lxxiv) y+1/2, z, x+1/2; (lxxv) x−1/2, y−1, −z+1/2; (lxxvi) x−1/2, y, −z+1/2; (lxxvii) x+1/2, y, −z+1/2; (lxxviii) −z−1/2, x−1, y+1/2; (lxxix) −z−1/2, x, y+1/2; (lxxx) −z+1/2, x, y+1/2; (lxxxi) y−1/2, −z−1, x+1/2; (lxxxii) y−1/2, −z, x+1/2; (lxxxiii) y+1/2, −z, x+1/2; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) z, x+1, y; (lxxxviii) z+1, x+1, y; (lxxxix) y−1, z−1, x; (xc) y−1, z, x; (xci) x−1, y−1, −z; (xcii) x−1, y, −z; (xciii) −z, x−1, y; (xciv) −z+1, x, y; (xcv) y, −z+1, x; (xcvi) y+1, −z+1, x; (xcvii) −z, −x, −y+1; (xcviii) −y, −z, −x+1; (xcix) −x, −y, z+1; (100) z, −x, −y+1; (101) −y, z, −x+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x−1, −y, −z+1; (105) −x, −y+1, −z+1; (106) z−1, −x, −y+1; (107) z, −x+1, −y+1.

(S4P35_phase_1)

Crystal data

O8.00P2Pb3.00	Z = 3
Mr = 811.54	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.4274 (3) Å	Particle morphology: plate
c = 19.9933 (14) Å	irregular, 6 × 6 mm
V = 510.03 (5) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.045	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 87.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.40 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 140.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 327.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.036	37 parameters
Rexp = 0.027	9 restraints
R(F^2) = 0.17911	(Δ/σ)max = 0.04
χ^2 = 1.742	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.93366 2: -0.520676 3: 0.794177 4: -0.211403 5: 0.364393 6: -0.181536 7: 0.230485 8: -0.103568 9: 0.130506 10: -5.480710E-0211: 4.592010E-0212: 2.853460E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92859 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
PB1	0.0	0.0	0.0	0.0162 (17)*
PB2	0.0	0.034 (3)	0.20992 (19)	0.0162 (17)*	0.16667
P	0.0	0.0	0.4042 (3)	0.0097 (16)*
O1	0.013 (2)	−0.013 (2)	0.3287 (3)	0.0154 (13)*	0.3333
O2	−0.142 (2)	0.1652 (19)	0.43011 (18)	0.0154 (13)*	0.5

Geometric parameters (Å, º)

PB1—PB2	4.201 (4)	P—PB2^lxxii	4.193 (5)
PB1—PB2^i	4.201 (4)	P—PB2^lxxiii	4.072 (11)
PB1—PB2^ii	4.201 (4)	P—PB2^lxxiv	4.311 (10)
PB1—PB2^iii	4.201 (4)	P—PB2^lxxv	4.072 (11)
PB1—PB2^iv	4.201 (4)	P—PB2^lxxvi	4.193 (5)
PB1—PB2^v	4.201 (4)	P—PB2^lxxvii	4.311 (10)
PB1—PB2^vi	4.201 (4)	P—PB2^lxxviii	4.193 (5)
PB1—PB2^vii	4.201 (4)	P—PB2^lxxix	4.311 (10)
PB1—PB2^viii	4.201 (4)	P—PB2^lxxx	4.072 (11)
PB1—PB2^ix	4.201 (4)	P—PB2^lxxxi	4.311 (10)
PB1—PB2^x	4.201 (4)	P—PB2^lxxxii	4.072 (11)
PB1—PB2^xi	4.201 (4)	P—PB2^lxxxiii	4.193 (5)
PB1—PB2^xii	3.993 (2)	P—P^lxxxiv	3.830 (11)
PB1—PB2^xiii	3.865 (10)	P—P^li	4.225 (8)
PB1—PB2^xiv	4.116 (10)	P—P^lii	4.225 (8)
PB1—PB2^xv	4.116 (10)	P—P^liii	4.225 (8)
PB1—PB2^xvi	3.993 (2)	P—O1	1.515 (6)
PB1—PB2^xvii	3.865 (10)	P—O1^i	1.515 (6)
PB1—PB2^xviii	3.865 (10)	P—O1^ii	1.515 (6)
PB1—PB2^xix	4.116 (10)	P—O1^li	3.461 (11)
PB1—PB2^xx	3.993 (2)	P—O1^lii	3.29 (2)
PB1—PB2^xxi	3.865 (10)	P—O1^liii	3.461 (11)
PB1—PB2^xxii	3.993 (2)	P—O1^liv	3.461 (11)
PB1—PB2^xxiii	4.116 (10)	P—O1^lv	3.461 (11)
PB1—PB2^xxiv	4.116 (10)	P—O1^lvi	3.29 (2)
PB1—PB2^xxv	3.865 (10)	P—O1^lvii	3.29 (2)
PB1—PB2^xxvi	3.993 (2)	P—O1^lviii	3.461 (11)
PB1—PB2^xxvii	3.993 (2)	P—O1^lix	3.461 (11)
PB1—PB2^xxviii	4.116 (10)	P—O2^lxxxv	4.230 (7)
PB1—PB2^xxix	3.865 (10)	P—O2	1.536 (4)
PB1—PB2^xxx	4.116 (10)	P—O2^lxxxvi	4.310 (7)
PB1—PB2^xxxi	3.865 (10)	P—O2^i	1.536 (4)
PB1—PB2^xxxii	3.993 (2)	P—O2^lxxxvii	4.310 (7)
PB1—PB2^xxxiii	3.865 (10)	P—O2^lxxxviii	4.230 (7)
PB1—PB2^xxxiv	3.993 (2)	P—O2^lxxxix	4.310 (7)
PB1—PB2^xxxv	4.116 (10)	P—O2^xc	4.230 (7)
PB1—PB2^xxxvi	3.993 (2)	P—O2^ii	1.536 (4)
PB1—PB2^xxxvii	4.116 (10)	P—O2^xci	4.230 (7)
PB1—PB2^xxxviii	3.865 (10)	P—O2^xcii	4.310 (7)
PB1—PB2^xxxix	4.116 (10)	P—O2^iii	1.536 (4)
PB1—PB2^xl	3.993 (2)	P—O2^xciii	4.310 (7)
PB1—PB2^xli	3.865 (10)	P—O2^iv	1.536 (4)
PB1—PB2^xlii	3.993 (2)	P—O2^xciv	4.230 (7)
PB1—PB2^xliii	3.865 (10)	P—O2^v	1.536 (4)
PB1—PB2^xliv	4.116 (10)	P—O2^xcv	4.230 (7)
PB1—PB2^xlv	3.865 (10)	P—O2^xcvi	4.310 (7)
PB1—PB2^xlvi	4.116 (10)	P—O2^lxxxiv	3.614 (7)
PB1—PB2^xlvii	3.993 (2)	P—O2^xcvii	3.614 (7)
PB1—P^xii	3.439 (2)	P—O2^xcviii	3.614 (7)
PB1—P^xiii	3.439 (2)	P—O2^xcix	3.614 (7)
PB1—P^xiv	3.439 (2)	P—O2^100	3.614 (7)
PB1—P^xxx	3.439 (2)	P—O2^101	3.614 (7)
PB1—P^xxxi	3.439 (2)	P—O2^li	4.354 (9)
PB1—P^xxxii	3.439 (2)	P—O2^liii	4.275 (8)
PB1—O1^xii	3.074 (10)	P—O2^liv	4.275 (8)
PB1—O1^xiii	3.26 (2)	P—O2^lv	4.354 (9)
PB1—O1^xiv	3.074 (10)	P—O2^lviii	4.275 (8)
PB1—O1^xv	3.074 (10)	P—O2^lix	4.354 (9)
PB1—O1^xvi	3.074 (10)	P—O2^lx	4.354 (9)
PB1—O1^xvii	3.26 (2)	P—O2^lxi	4.275 (8)
PB1—O1^xviii	3.26 (2)	P—O2^lxii	4.275 (8)
PB1—O1^xix	3.074 (10)	P—O2^lxiii	4.354 (9)
PB1—O1^xx	3.074 (10)	P—O2^lxiv	4.354 (9)
PB1—O1^xxx	3.074 (10)	P—O2^lxv	4.275 (8)
PB1—O1^xxxi	3.26 (2)	O1—PB1^xlviii	3.074 (10)
PB1—O1^xxxii	3.074 (10)	O1—PB1^xlix	3.26 (2)
PB1—O1^xxxiii	3.26 (2)	O1—PB1^l	3.074 (10)
PB1—O1^xxxiv	3.074 (10)	O1—PB2	2.393 (7)
PB1—O1^xxxv	3.074 (10)	O1—PB2^i	2.385 (7)
PB1—O1^xxxvi	3.074 (10)	O1—PB2^ii	2.377 (7)
PB1—O1^xxxvii	3.074 (10)	O1—PB2^iii	2.385 (7)
PB1—O1^xxxviii	3.26 (2)	O1—PB2^iv	2.393 (7)
PB1—O2^xiii	2.569 (4)	O1—PB2^v	2.377 (7)
PB1—O2^xvii	2.569 (4)	O1—PB2^li	4.096 (9)
PB1—O2^xviii	2.569 (4)	O1—PB2^lii	4.075 (19)
PB1—O2^xxi	2.569 (4)	O1—PB2^liii	3.972 (12)
PB1—O2^xxv	2.569 (4)	O1—PB2^liv	3.977 (13)
PB1—O2^xxix	2.569 (4)	O1—PB2^lv	3.955 (17)
PB1—O2^xxxi	2.569 (4)	O1—PB2^lvi	4.221 (15)
PB1—O2^xxxiii	2.569 (4)	O1—PB2^lvii	4.225 (15)
PB1—O2^xxxviii	2.569 (4)	O1—PB2^lviii	3.83 (2)
PB1—O2^xli	2.569 (4)	O1—PB2^lix	4.105 (11)
PB1—O2^xliii	2.569 (4)	O1—PB2^lxvi	4.221 (15)
PB1—O2^xlv	2.569 (4)	O1—PB2^lx	3.955 (17)
PB2—PB1	4.201 (4)	O1—PB2^lxi	3.977 (13)
PB2—PB1^xlviii	4.116 (10)	O1—PB2^lxii	3.972 (12)
PB2—PB1^xlix	3.865 (10)	O1—PB2^lxvii	4.075 (19)
PB2—PB1^l	3.993 (2)	O1—PB2^lxiii	4.096 (9)
PB2—PB2^i	0.32 (3)	O1—PB2^lxiv	4.105 (11)
PB2—PB2^ii	0.32 (3)	O1—PB2^lxv	3.83 (2)
PB2—PB2^iii	0.184 (14)	O1—PB2^lxviii	4.225 (15)
PB2—PB2^iv	0.184 (14)	O1—P	1.515 (6)
PB2—PB2^v	0.37 (3)	O1—P^li	3.461 (11)
PB2—PB2^xxx	3.87 (2)	O1—P^lii	3.29 (2)
PB2—PB2^xxxi	3.31 (2)	O1—P^liii	3.461 (11)
PB2—PB2^xxxii	3.598 (5)	O1—O1^i	0.22 (4)
PB2—PB2^xxxiii	3.584 (4)	O1—O1^ii	0.22 (4)
PB2—PB2^xxxiv	3.441 (11)	O1—O1^li	3.27 (2)
PB2—PB2^xxxv	3.721 (12)	O1—O1^lii	2.89 (4)
PB2—PB2^xxxvi	3.721 (12)	O1—O1^liii	3.27 (2)
PB2—PB2^xxxvii	3.584 (4)	O1—O1^liv	3.26 (2)
PB2—PB2^xxxviii	3.441 (11)	O1—O1^lv	3.079 (10)
PB2—PB2^xxxix	3.86 (2)	O1—O1^lvi	3.079 (10)
PB2—PB2^xl	3.451 (10)	O1—O1^lvii	3.079 (10)
PB2—PB2^xli	3.451 (10)	O1—O1^lviii	3.079 (10)
PB2—PB2^xlii	3.730 (13)	O1—O1^lix	3.26 (2)
PB2—PB2^xliii	3.30 (2)	O1—O2	2.565 (14)
PB2—PB2^xliv	3.730 (13)	O1—O2^i	2.460 (8)
PB2—PB2^xlv	3.579 (4)	O1—O2^ii	2.454 (8)
PB2—PB2^xlvi	3.579 (4)	O1—O2^iii	2.460 (8)
PB2—PB2^xlvii	3.579 (4)	O1—O2^iv	2.565 (14)
PB2—P	3.889 (8)	O1—O2^v	2.454 (8)
PB2—P^xii	4.193 (5)	O1—O2^li	3.341 (10)
PB2—P^xiii	4.311 (10)	O1—O2^liii	3.237 (9)
PB2—P^xiv	4.072 (11)	O1—O2^liv	3.318 (17)
PB2—P^li	3.3100 (19)	O1—O2^lv	3.243 (17)
PB2—P^lii	3.458 (12)	O1—O2^lviii	3.141 (19)
PB2—P^liii	3.155 (12)	O1—O2^lix	3.42 (2)
PB2—O1	2.393 (7)	O1—O2^lx	3.243 (17)
PB2—O1^i	2.377 (7)	O1—O2^lxi	3.318 (17)
PB2—O1^ii	2.385 (7)	O1—O2^lxii	3.237 (9)
PB2—O1^li	4.096 (9)	O1—O2^lxiii	3.341 (10)
PB2—O1^lii	4.075 (19)	O1—O2^lxiv	3.42 (2)
PB2—O1^liii	3.972 (12)	O1—O2^lxv	3.141 (19)
PB2—O1^liv	4.105 (11)	O2—PB1^xlix	2.569 (4)
PB2—O1^lv	4.225 (15)	O2—PB2^li	2.918 (13)
PB2—O1^lvi	3.83 (2)	O2—PB2^liii	2.614 (12)
PB2—O1^lvii	3.955 (17)	O2—PB2^liv	2.649 (17)
PB2—O1^lviii	4.221 (15)	O2—PB2^lvi	2.888 (17)
PB2—O1^lix	3.977 (13)	O2—PB2^lvii	2.931 (13)
PB2—O2^xiii	2.922 (8)	O2—PB2^lix	2.629 (12)
PB2—O2^xvii	2.731 (9)	O2—PB2^lxvi	3.011 (17)
PB2—O2^xviii	2.834 (4)	O2—PB2^lxi	2.526 (18)
PB2—O2^xxi	2.826 (4)	O2—PB2^lxii	2.737 (12)
PB2—O2^xxv	2.926 (8)	O2—PB2^lxiii	2.795 (12)
PB2—O2^xxix	2.735 (9)	O2—PB2^lxiv	2.751 (12)
PB2—O2^li	2.918 (13)	O2—PB2^lxviii	2.809 (13)
PB2—O2^liii	2.614 (12)	O2—PB2^xlix	2.922 (8)
PB2—O2^liv	2.629 (12)	O2—PB2^lxx	2.834 (4)
PB2—O2^lv	2.931 (13)	O2—PB2^lxxiii	2.731 (9)
PB2—O2^lviii	2.888 (17)	O2—PB2^lxxvi	2.826 (4)
PB2—O2^lix	2.649 (17)	O2—PB2^lxxix	2.926 (8)
PB2—O2^lx	3.011 (17)	O2—PB2^lxxxii	2.735 (9)
PB2—O2^lxi	2.526 (18)	O2—P^102	4.310 (7)
PB2—O2^lxii	2.795 (12)	O2—P	1.536 (4)
PB2—O2^lxiii	2.737 (12)	O2—P^103	4.230 (7)
PB2—O2^lxiv	2.751 (12)	O2—P^lxxxiv	3.614 (7)
PB2—O2^lxv	2.809 (13)	O2—P^li	4.354 (9)
P—PB1^xlviii	3.439 (2)	O2—P^liii	4.275 (8)
P—PB1^xlix	3.439 (2)	O2—O1	2.565 (14)
P—PB1^l	3.439 (2)	O2—O1^i	2.454 (8)
P—PB2	3.889 (8)	O2—O1^ii	2.460 (8)
P—PB2^i	3.889 (8)	O2—O1^li	3.341 (10)
P—PB2^ii	3.889 (8)	O2—O1^liii	3.237 (9)
P—PB2^iii	3.889 (8)	O2—O1^liv	3.42 (2)
P—PB2^iv	3.889 (8)	O2—O1^lvi	3.141 (19)
P—PB2^v	3.889 (8)	O2—O1^lvii	3.243 (17)
P—PB2^li	3.3100 (19)	O2—O1^lix	3.318 (17)
P—PB2^lii	3.458 (12)	O2—O2^i	2.504 (6)
P—PB2^liii	3.155 (12)	O2—O2^lxxxvii	2.927 (7)
P—PB2^liv	3.155 (12)	O2—O2^xc	2.927 (7)
P—PB2^lv	3.3100 (19)	O2—O2^ii	2.504 (6)
P—PB2^lvi	3.458 (12)	O2—O2^xcii	2.988 (12)
P—PB2^lvii	3.458 (12)	O2—O2^iii	2.439 (12)
P—PB2^lviii	3.155 (12)	O2—O2^iv	0.13 (2)
P—PB2^lix	3.3100 (19)	O2—O2^v	2.565 (12)
P—PB2^lxvi	3.458 (12)	O2—O2^xcv	2.863 (12)
P—PB2^lx	3.3100 (19)	O2—O2^104	4.376 (15)
P—PB2^lxi	3.155 (12)	O2—O2^lxxxiv	4.022 (7)
P—PB2^lxii	3.155 (12)	O2—O2^105	4.218 (14)
P—PB2^lxvii	3.458 (12)	O2—O2^xcvii	3.147 (7)
P—PB2^lxiii	3.3100 (19)	O2—O2^xcviii	3.147 (7)
P—PB2^lxiv	3.3100 (19)	O2—O2^xcix	3.197 (11)
P—PB2^lxv	3.155 (12)	O2—O2^106	4.296 (5)
P—PB2^lxviii	3.458 (12)	O2—O2^100	4.020 (7)
P—PB2^xlviii	4.072 (11)	O2—O2^107	4.296 (5)
P—PB2^xlix	4.311 (10)	O2—O2^101	3.098 (10)
P—PB2^l	4.193 (5)	O2—O2^liv	4.223 (7)
P—PB2^lxix	4.311 (10)	O2—O2^lix	4.223 (7)
P—PB2^lxx	4.193 (5)	O2—O2^lxi	4.180 (9)
P—PB2^lxxi	4.072 (11)	O2—O2^lxiv	4.267 (10)
PB2^i—PB2—PB2^ii	60.0	O1^ii—P—O2	107.5 (5)
PB2^i—PB2—PB2^iii	90.0000 (2)	O1^ii—P—O2^i	107.1 (5)
PB2^i—PB2—PB2^iv	30.0000 (9)	O1^ii—P—O2^ii	114.4 (9)
PB2^i—PB2—PB2^v	30.0	O1^ii—P—O2^iii	114.4 (9)
PB2^ii—PB2—PB2^iii	30.0000 (9)	O1^ii—P—O2^iv	107.1 (5)
PB2^ii—PB2—PB2^iv	90.0000 (2)	O1^ii—P—O2^v	107.5 (5)
PB2^ii—PB2—PB2^v	30.0	O2—P—O2^i	109.2 (2)
PB2^iii—PB2—PB2^iv	120.0000 (19)	O2—P—O2^ii	109.2 (2)
PB2^iii—PB2—PB2^v	60.0000 (4)	O2—P—O2^iii	105.1 (7)
PB2^iv—PB2—PB2^v	60.0000 (4)	O2—P—O2^iv	4.7 (8)
O1—P—O1^i	8.2 (14)	O2—P—O2^v	113.2 (7)
O1—P—O1^ii	8.2 (14)	O2^i—P—O2^ii	109.2 (2)
O1—P—O2	114.4 (9)	O2^i—P—O2^iii	113.2 (7)
O1—P—O2^i	107.5 (5)	O2^i—P—O2^iv	105.1 (7)
O1—P—O2^ii	107.1 (5)	O2^i—P—O2^v	4.7 (8)
O1—P—O2^iii	107.5 (5)	O2^ii—P—O2^iii	4.7 (8)
O1—P—O2^iv	114.4 (9)	O2^ii—P—O2^iv	113.2 (7)
O1—P—O2^v	107.1 (5)	O2^ii—P—O2^v	105.1 (7)
O1^i—P—O1^ii	8.2 (14)	O2^iii—P—O2^iv	109.2 (2)
O1^i—P—O2	107.1 (5)	O2^iii—P—O2^v	109.2 (2)
O1^i—P—O2^i	114.4 (9)	O2^iv—P—O2^v	109.2 (2)
O1^i—P—O2^ii	107.5 (5)	P—O1—O1^i	85.9 (7)
O1^i—P—O2^iii	107.1 (5)	P—O1—O1^ii	85.9 (7)
O1^i—P—O2^iv	107.5 (5)	O1^i—O1—O1^ii	60.0
O1^i—P—O2^v	114.4 (9)	P—O2—O2^iv	87.7 (4)

Symmetry codes: (i) −y, x−y, z; (ii) y−x, −x, z; (iii) y−x, y, z; (iv) −y, −x, z; (v) x, x−y, z; (vi) −x, −y, −z; (vii) y, y−x, −z; (viii) x−y, x, −z; (ix) x−y, −y, −z; (x) y, x, −z; (xi) −x, y−x, −z; (xii) x−2/3, y−1/3, z−1/3; (xiii) x+1/3, y−1/3, z−1/3; (xiv) x+1/3, y+2/3, z−1/3; (xv) −y−2/3, x−y−1/3, z−1/3; (xvi) −y+1/3, x−y−1/3, z−1/3; (xvii) −y+1/3, x−y+2/3, z−1/3; (xviii) y−x−2/3, −x−1/3, z−1/3; (xix) y−x+1/3, −x−1/3, z−1/3; (xx) y−x+1/3, −x+2/3, z−1/3; (xxi) y−x−2/3, y−1/3, z−1/3; (xxii) y−x+1/3, y−1/3, z−1/3; (xxiii) y−x+1/3, y+2/3, z−1/3; (xxiv) −y−2/3, −x−1/3, z−1/3; (xxv) −y+1/3, −x−1/3, z−1/3; (xxvi) −y+1/3, −x+2/3, z−1/3; (xxvii) x−2/3, x−y−1/3, z−1/3; (xxviii) x+1/3, x−y−1/3, z−1/3; (xxix) x+1/3, x−y+2/3, z−1/3; (xxx) −x−2/3, −y−1/3, −z+2/3; (xxxi) −x−2/3, −y+2/3, −z+2/3; (xxxii) −x+1/3, −y+2/3, −z+2/3; (xxxiii) y−2/3, y−x−1/3, −z+2/3; (xxxiv) y−2/3, y−x+2/3, −z+2/3; (xxxv) y+1/3, y−x+2/3, −z+2/3; (xxxvi) x−y−2/3, x−1/3, −z+2/3; (xxxvii) x−y−2/3, x+2/3, −z+2/3; (xxxviii) x−y+1/3, x+2/3, −z+2/3; (xxxix) x−y−2/3, −y−1/3, −z+2/3; (xl) x−y−2/3, −y+2/3, −z+2/3; (xli) x−y+1/3, −y+2/3, −z+2/3; (xlii) y−2/3, x−1/3, −z+2/3; (xliii) y−2/3, x+2/3, −z+2/3; (xliv) y+1/3, x+2/3, −z+2/3; (xlv) −x−2/3, y−x−1/3, −z+2/3; (xlvi) −x−2/3, y−x+2/3, −z+2/3; (xlvii) −x+1/3, y−x+2/3, −z+2/3; (xlviii) x−1/3, y−2/3, z+1/3; (xlix) x−1/3, y+1/3, z+1/3; (l) x+2/3, y+1/3, z+1/3; (li) −x−1/3, −y−2/3, −z+1/3; (lii) −x+2/3, −y−2/3, −z+1/3; (liii) −x+2/3, −y+1/3, −z+1/3; (liv) y−1/3, y−x−2/3, −z+1/3; (lv) y+2/3, y−x−2/3, −z+1/3; (lvi) y+2/3, y−x+1/3, −z+1/3; (lvii) x−y−1/3, x−2/3, −z+1/3; (lviii) x−y+2/3, x−2/3, −z+1/3; (lix) x−y+2/3, x+1/3, −z+1/3; (lx) x−y+2/3, −y−2/3, −z+1/3; (lxi) x−y+2/3, −y+1/3, −z+1/3; (lxii) y−1/3, x−2/3, −z+1/3; (lxiii) y+2/3, x+1/3, −z+1/3; (lxiv) −x−1/3, y−x−2/3, −z+1/3; (lxv) −x+2/3, y−x−2/3, −z+1/3; (lxvi) x−y−1/3, −y−2/3, −z+1/3; (lxvii) y+2/3, x−2/3, −z+1/3; (lxviii) −x+2/3, y−x+1/3, −z+1/3; (lxix) −y−1/3, x−y−2/3, z+1/3; (lxx) −y−1/3, x−y+1/3, z+1/3; (lxxi) −y+2/3, x−y+1/3, z+1/3; (lxxii) y−x−1/3, −x−2/3, z+1/3; (lxxiii) y−x−1/3, −x+1/3, z+1/3; (lxxiv) y−x+2/3, −x+1/3, z+1/3; (lxxv) y−x−1/3, y−2/3, z+1/3; (lxxvi) y−x−1/3, y+1/3, z+1/3; (lxxvii) y−x+2/3, y+1/3, z+1/3; (lxxviii) −y−1/3, −x−2/3, z+1/3; (lxxix) −y−1/3, −x+1/3, z+1/3; (lxxx) −y+2/3, −x+1/3, z+1/3; (lxxxi) x−1/3, x−y−2/3, z+1/3; (lxxxii) x−1/3, x−y+1/3, z+1/3; (lxxxiii) x+2/3, x−y+1/3, z+1/3; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) −y, x−y+1, z; (lxxxviii) −y+1, x−y+1, z; (lxxxix) y−x−1, −x−1, z; (xc) y−x−1, −x, z; (xci) y−x−1, y−1, z; (xcii) y−x−1, y, z; (xciii) −y, −x−1, z; (xciv) −y+1, −x, z; (xcv) x, x−y+1, z; (xcvi) x+1, x−y+1, z; (xcvii) y, y−x, −z+1; (xcviii) x−y, x, −z+1; (xcix) x−y, −y, −z+1; (100) y, x, −z+1; (101) −x, y−x, −z+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x−1, −y, −z+1; (105) −x, −y+1, −z+1; (106) y−1, x, −z+1; (107) y, x+1, −z+1.

(S4P35_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8984 (6) Å	T = 298 K
c = 2.8288 (10) Å	Particle morphology: Pressure cell anvil material
V = 20.58 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.045	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 87.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.40 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 140.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 327.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.036	37 parameters
Rexp = 0.027	9 restraints
R(F^2) = 0.17911	(Δ/σ)max = 0.04
χ^2 = 1.742	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.93366 2: -0.520676 3: 0.794177 4: -0.211403 5: 0.364393 6: -0.181536 7: 0.230485 8: -0.103568 9: 0.130506 10: -5.480710E-0211: 4.592010E-0212: 2.853460E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92859 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.201 (4)	P—PB2	4.193 (5)
PB1—PB2^i	4.201 (4)	P—PB2	4.072 (11)
PB1—PB2^ii	4.201 (4)	P—PB2	4.311 (10)
PB1—PB2^iii	4.201 (4)	P—PB2	4.072 (11)
PB1—PB2^iv	4.201 (4)	P—PB2	4.193 (5)
PB1—PB2^v	4.201 (4)	P—PB2	4.311 (10)
PB1—PB2	4.201 (4)	P—PB2	4.193 (5)
PB1—PB2	4.201 (4)	P—PB2	4.311 (10)
PB1—PB2	4.201 (4)	P—PB2	4.072 (11)
PB1—PB2	4.201 (4)	P—PB2	4.311 (10)
PB1—PB2	4.201 (4)	P—PB2	4.072 (11)
PB1—PB2	4.201 (4)	P—PB2	4.193 (5)
PB1—PB2	3.993 (2)	P—P	3.830 (11)
PB1—PB2	3.865 (10)	P—P	4.225 (8)
PB1—PB2	4.116 (10)	P—P	4.225 (8)
PB1—PB2	4.116 (10)	P—P	4.225 (8)
PB1—PB2	3.993 (2)	P—O1	1.515 (6)
PB1—PB2	3.865 (10)	P—O1^i	1.515 (6)
PB1—PB2	3.865 (10)	P—O1^ii	1.515 (6)
PB1—PB2	4.116 (10)	P—O1	3.461 (11)
PB1—PB2	3.993 (2)	P—O1	3.29 (2)
PB1—PB2	3.865 (10)	P—O1	3.461 (11)
PB1—PB2	3.993 (2)	P—O1	3.461 (11)
PB1—PB2	4.116 (10)	P—O1	3.461 (11)
PB1—PB2	4.116 (10)	P—O1	3.29 (2)
PB1—PB2	3.865 (10)	P—O1	3.29 (2)
PB1—PB2	3.993 (2)	P—O1	3.461 (11)
PB1—PB2	3.993 (2)	P—O1	3.461 (11)
PB1—PB2	4.116 (10)	P—O2^vi	4.230 (7)
PB1—PB2	3.865 (10)	P—O2	1.536 (4)
PB1—PB2	4.116 (10)	P—O2^vii	4.310 (7)
PB1—PB2	3.865 (10)	P—O2^i	1.536 (4)
PB1—PB2	3.993 (2)	P—O2^viii	4.310 (7)
PB1—PB2	3.865 (10)	P—O2^ix	4.230 (7)
PB1—PB2	3.993 (2)	P—O2^x	4.310 (7)
PB1—PB2	4.116 (10)	P—O2^xi	4.230 (7)
PB1—PB2	3.993 (2)	P—O2^ii	1.536 (4)
PB1—PB2	4.116 (10)	P—O2^xii	4.230 (7)
PB1—PB2	3.865 (10)	P—O2^xiii	4.310 (7)
PB1—PB2	4.116 (10)	P—O2^iii	1.536 (4)
PB1—PB2	3.993 (2)	P—O2^xiv	4.310 (7)
PB1—PB2	3.865 (10)	P—O2^iv	1.536 (4)
PB1—PB2	3.993 (2)	P—O2^xv	4.230 (7)
PB1—PB2	3.865 (10)	P—O2^v	1.536 (4)
PB1—PB2	4.116 (10)	P—O2^xvi	4.230 (7)
PB1—PB2	3.865 (10)	P—O2^xvii	4.310 (7)
PB1—PB2	4.116 (10)	P—O2	3.614 (7)
PB1—PB2	3.993 (2)	P—O2	3.614 (7)
PB1—P	3.439 (2)	P—O2	3.614 (7)
PB1—P	3.439 (2)	P—O2	3.614 (7)
PB1—P	3.439 (2)	P—O2	3.614 (7)
PB1—P	3.439 (2)	P—O2	3.614 (7)
PB1—P	3.439 (2)	P—O2	4.354 (9)
PB1—P	3.439 (2)	P—O2	4.275 (8)
PB1—O1	3.074 (10)	P—O2	4.275 (8)
PB1—O1	3.26 (2)	P—O2	4.354 (9)
PB1—O1	3.074 (10)	P—O2	4.275 (8)
PB1—O1	3.074 (10)	P—O2	4.354 (9)
PB1—O1	3.074 (10)	P—O2	4.354 (9)
PB1—O1	3.26 (2)	P—O2	4.275 (8)
PB1—O1	3.26 (2)	P—O2	4.275 (8)
PB1—O1	3.074 (10)	P—O2	4.354 (9)
PB1—O1	3.074 (10)	P—O2	4.354 (9)
PB1—O1	3.074 (10)	P—O2	4.275 (8)
PB1—O1	3.26 (2)	O1—PB1	3.074 (10)
PB1—O1	3.074 (10)	O1—PB1	3.26 (2)
PB1—O1	3.26 (2)	O1—PB1	3.074 (10)
PB1—O1	3.074 (10)	O1—PB2	2.393 (7)
PB1—O1	3.074 (10)	O1—PB2^i	2.385 (7)
PB1—O1	3.074 (10)	O1—PB2^ii	2.377 (7)
PB1—O1	3.074 (10)	O1—PB2^iii	2.385 (7)
PB1—O1	3.26 (2)	O1—PB2^iv	2.393 (7)
PB1—O2	2.569 (4)	O1—PB2^v	2.377 (7)
PB1—O2	2.569 (4)	O1—PB2	4.096 (9)
PB1—O2	2.569 (4)	O1—PB2	4.075 (19)
PB1—O2	2.569 (4)	O1—PB2	3.972 (12)
PB1—O2	2.569 (4)	O1—PB2	3.977 (13)
PB1—O2	2.569 (4)	O1—PB2	3.955 (17)
PB1—O2	2.569 (4)	O1—PB2	4.221 (15)
PB1—O2	2.569 (4)	O1—PB2	4.225 (15)
PB1—O2	2.569 (4)	O1—PB2	3.83 (2)
PB1—O2	2.569 (4)	O1—PB2	4.105 (11)
PB1—O2	2.569 (4)	O1—PB2	4.221 (15)
PB1—O2	2.569 (4)	O1—PB2	3.955 (17)
PB2—PB1	4.201 (4)	O1—PB2	3.977 (13)
PB2—PB1	4.116 (10)	O1—PB2	3.972 (12)
PB2—PB1	3.865 (10)	O1—PB2	4.075 (19)
PB2—PB1	3.993 (2)	O1—PB2	4.096 (9)
PB2—PB2^i	0.32 (3)	O1—PB2	4.105 (11)
PB2—PB2^ii	0.32 (3)	O1—PB2	3.83 (2)
PB2—PB2^iii	0.184 (14)	O1—PB2	4.225 (15)
PB2—PB2^iv	0.184 (14)	O1—P	1.515 (6)
PB2—PB2^v	0.37 (3)	O1—P	3.461 (11)
PB2—PB2	3.87 (2)	O1—P	3.29 (2)
PB2—PB2	3.31 (2)	O1—P	3.461 (11)
PB2—PB2	3.598 (5)	O1—O1^i	0.22 (4)
PB2—PB2	3.584 (4)	O1—O1^ii	0.22 (4)
PB2—PB2	3.441 (11)	O1—O1	3.27 (2)
PB2—PB2	3.721 (12)	O1—O1	2.89 (4)
PB2—PB2	3.721 (12)	O1—O1	3.27 (2)
PB2—PB2	3.584 (4)	O1—O1	3.26 (2)
PB2—PB2	3.441 (11)	O1—O1	3.079 (10)
PB2—PB2	3.86 (2)	O1—O1	3.079 (10)
PB2—PB2	3.451 (10)	O1—O1	3.079 (10)
PB2—PB2	3.451 (10)	O1—O1	3.079 (10)
PB2—PB2	3.730 (13)	O1—O1	3.26 (2)
PB2—PB2	3.30 (2)	O1—O2	2.565 (14)
PB2—PB2	3.730 (13)	O1—O2^i	2.460 (8)
PB2—PB2	3.579 (4)	O1—O2^ii	2.454 (8)
PB2—PB2	3.579 (4)	O1—O2^iii	2.460 (8)
PB2—PB2	3.579 (4)	O1—O2^iv	2.565 (14)
PB2—P	3.889 (8)	O1—O2^v	2.454 (8)
PB2—P	4.193 (5)	O1—O2	3.341 (10)
PB2—P	4.311 (10)	O1—O2	3.237 (9)
PB2—P	4.072 (11)	O1—O2	3.318 (17)
PB2—P	3.3100 (19)	O1—O2	3.243 (17)
PB2—P	3.458 (12)	O1—O2	3.141 (19)
PB2—P	3.155 (12)	O1—O2	3.42 (2)
PB2—O1	2.393 (7)	O1—O2	3.243 (17)
PB2—O1^i	2.377 (7)	O1—O2	3.318 (17)
PB2—O1^ii	2.385 (7)	O1—O2	3.237 (9)
PB2—O1	4.096 (9)	O1—O2	3.341 (10)
PB2—O1	4.075 (19)	O1—O2	3.42 (2)
PB2—O1	3.972 (12)	O1—O2	3.141 (19)
PB2—O1	4.105 (11)	O2—PB1	2.569 (4)
PB2—O1	4.225 (15)	O2—PB2	2.918 (13)
PB2—O1	3.83 (2)	O2—PB2	2.614 (12)
PB2—O1	3.955 (17)	O2—PB2	2.649 (17)
PB2—O1	4.221 (15)	O2—PB2	2.888 (17)
PB2—O1	3.977 (13)	O2—PB2	2.931 (13)
PB2—O2	2.922 (8)	O2—PB2	2.629 (12)
PB2—O2	2.731 (9)	O2—PB2	3.011 (17)
PB2—O2	2.834 (4)	O2—PB2	2.526 (18)
PB2—O2	2.826 (4)	O2—PB2	2.737 (12)
PB2—O2	2.926 (8)	O2—PB2	2.795 (12)
PB2—O2	2.735 (9)	O2—PB2	2.751 (12)
PB2—O2	2.918 (13)	O2—PB2	2.809 (13)
PB2—O2	2.614 (12)	O2—PB2	2.922 (8)
PB2—O2	2.629 (12)	O2—PB2	2.834 (4)
PB2—O2	2.931 (13)	O2—PB2	2.731 (9)
PB2—O2	2.888 (17)	O2—PB2	2.826 (4)
PB2—O2	2.649 (17)	O2—PB2	2.926 (8)
PB2—O2	3.011 (17)	O2—PB2	2.735 (9)
PB2—O2	2.526 (18)	O2—P^xviii	4.310 (7)
PB2—O2	2.795 (12)	O2—P	1.536 (4)
PB2—O2	2.737 (12)	O2—P^xix	4.230 (7)
PB2—O2	2.751 (12)	O2—P	3.614 (7)
PB2—O2	2.809 (13)	O2—P	4.354 (9)
P—PB1	3.439 (2)	O2—P	4.275 (8)
P—PB1	3.439 (2)	O2—O1	2.565 (14)
P—PB1	3.439 (2)	O2—O1^i	2.454 (8)
P—PB2	3.889 (8)	O2—O1^ii	2.460 (8)
P—PB2^i	3.889 (8)	O2—O1	3.341 (10)
P—PB2^ii	3.889 (8)	O2—O1	3.237 (9)
P—PB2^iii	3.889 (8)	O2—O1	3.42 (2)
P—PB2^iv	3.889 (8)	O2—O1	3.141 (19)
P—PB2^v	3.889 (8)	O2—O1	3.243 (17)
P—PB2	3.3100 (19)	O2—O1	3.318 (17)
P—PB2	3.458 (12)	O2—O2^i	2.504 (6)
P—PB2	3.155 (12)	O2—O2^viii	2.927 (7)
P—PB2	3.155 (12)	O2—O2^xi	2.927 (7)
P—PB2	3.3100 (19)	O2—O2^ii	2.504 (6)
P—PB2	3.458 (12)	O2—O2^xiii	2.988 (12)
P—PB2	3.458 (12)	O2—O2^iii	2.439 (12)
P—PB2	3.155 (12)	O2—O2^iv	0.13 (2)
P—PB2	3.3100 (19)	O2—O2^v	2.565 (12)
P—PB2	3.458 (12)	O2—O2^xvi	2.863 (12)
P—PB2	3.3100 (19)	O2—O2	4.376 (15)
P—PB2	3.155 (12)	O2—O2	4.022 (7)
P—PB2	3.155 (12)	O2—O2	4.218 (14)
P—PB2	3.458 (12)	O2—O2	3.147 (7)
P—PB2	3.3100 (19)	O2—O2	3.147 (7)
P—PB2	3.3100 (19)	O2—O2	3.197 (11)
P—PB2	3.155 (12)	O2—O2	4.296 (5)
P—PB2	3.458 (12)	O2—O2	4.020 (7)
P—PB2	4.072 (11)	O2—O2	4.296 (5)
P—PB2	4.311 (10)	O2—O2	3.098 (10)
P—PB2	4.193 (5)	O2—O2	4.223 (7)
P—PB2	4.311 (10)	O2—O2	4.223 (7)
P—PB2	4.193 (5)	O2—O2	4.180 (9)
P—PB2	4.072 (11)	O2—O2	4.267 (10)
PB2^i—PB2—PB2^ii	60.0	O1^ii—P—O2	107.5 (5)
PB2^i—PB2—PB2^iii	90.0000 (2)	O1^ii—P—O2^i	107.1 (5)
PB2^i—PB2—PB2^iv	30.0000 (9)	O1^ii—P—O2^ii	114.4 (9)
PB2^i—PB2—PB2^v	30.0	O1^ii—P—O2^iii	114.4 (9)
PB2^ii—PB2—PB2^iii	30.0000 (9)	O1^ii—P—O2^iv	107.1 (5)
PB2^ii—PB2—PB2^iv	90.0000 (2)	O1^ii—P—O2^v	107.5 (5)
PB2^ii—PB2—PB2^v	30.0	O2—P—O2^i	109.2 (2)
PB2^iii—PB2—PB2^iv	120.0000 (19)	O2—P—O2^ii	109.2 (2)
PB2^iii—PB2—PB2^v	60.0000 (4)	O2—P—O2^iii	105.1 (7)
PB2^iv—PB2—PB2^v	60.0000 (4)	O2—P—O2^iv	4.7 (8)
O1—P—O1^i	8.2 (14)	O2—P—O2^v	113.2 (7)
O1—P—O1^ii	8.2 (14)	O2^i—P—O2^ii	109.2 (2)
O1—P—O2	114.4 (9)	O2^i—P—O2^iii	113.2 (7)
O1—P—O2^i	107.5 (5)	O2^i—P—O2^iv	105.1 (7)
O1—P—O2^ii	107.1 (5)	O2^i—P—O2^v	4.7 (8)
O1—P—O2^iii	107.5 (5)	O2^ii—P—O2^iii	4.7 (8)
O1—P—O2^iv	114.4 (9)	O2^ii—P—O2^iv	113.2 (7)
O1—P—O2^v	107.1 (5)	O2^ii—P—O2^v	105.1 (7)
O1^i—P—O1^ii	8.2 (14)	O2^iii—P—O2^iv	109.2 (2)
O1^i—P—O2	107.1 (5)	O2^iii—P—O2^v	109.2 (2)
O1^i—P—O2^i	114.4 (9)	O2^iv—P—O2^v	109.2 (2)
O1^i—P—O2^ii	107.5 (5)	P—O1—O1^i	85.9 (7)
O1^i—P—O2^iii	107.1 (5)	P—O1—O1^ii	85.9 (7)
O1^i—P—O2^iv	107.5 (5)	O1^i—O1—O1^ii	60.0
O1^i—P—O2^v	114.4 (9)	P—O2—O2^iv	87.7 (4)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) x, y, −z; (iv) y−x, −x, z; (v) −y, x−y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) y−x, −x+1, −z; (ix) y−x+1, −x+1, −z; (x) −y−1, x−y−1, z; (xi) −y−1, x−y, z; (xii) x−1, y−1, −z; (xiii) x−1, y, −z; (xiv) y−x, −x−1, z; (xv) y−x+1, −x, z; (xvi) −y, x−y+1, −z; (xvii) −y+1, x−y+1, −z; (xviii) x−1, y, z; (xix) x, y+1, z.

(S4P35_phase_3)

Crystal data

Ni	anvil material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5433 (9) Å	Particle morphology: Component of pressure cell, not sample
V = 44.49 (1) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.587 Angstrom (no useful data), d > 3.73 Angstrom (no useful data)
Rp = 0.045	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 87.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 6.40 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 140.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 327.4 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.036	37 parameters
Rexp = 0.027	9 restraints
R(F^2) = 0.17911	(Δ/σ)max = 0.04
χ^2 = 1.742	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.93366 2: -0.520676 3: 0.794177 4: -0.211403 5: 0.364393 6: -0.181536 7: 0.230485 8: -0.103568 9: 0.130506 10: -5.480710E-0211: 4.592010E-0212: 2.853460E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.92859 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.201 (4)	P—PB2^lxxii	4.193 (5)
PB1—PB2^i	4.201 (4)	P—PB2^lxxiii	4.072 (11)
PB1—PB2^ii	4.201 (4)	P—PB2^lxxiv	4.311 (10)
PB1—PB2^iii	4.201 (4)	P—PB2^lxxv	4.072 (11)
PB1—PB2^iv	4.201 (4)	P—PB2^lxxvi	4.193 (5)
PB1—PB2^v	4.201 (4)	P—PB2^lxxvii	4.311 (10)
PB1—PB2^vi	4.201 (4)	P—PB2^lxxviii	4.193 (5)
PB1—PB2^vii	4.201 (4)	P—PB2^lxxix	4.311 (10)
PB1—PB2^viii	4.201 (4)	P—PB2^lxxx	4.072 (11)
PB1—PB2^ix	4.201 (4)	P—PB2^lxxxi	4.311 (10)
PB1—PB2^x	4.201 (4)	P—PB2^lxxxii	4.072 (11)
PB1—PB2^xi	4.201 (4)	P—PB2^lxxxiii	4.193 (5)
PB1—PB2^xii	3.993 (2)	P—P^lxxxiv	3.830 (11)
PB1—PB2^xiii	3.865 (10)	P—P^li	4.225 (8)
PB1—PB2^xiv	4.116 (10)	P—P^lii	4.225 (8)
PB1—PB2^xv	4.116 (10)	P—P^liii	4.225 (8)
PB1—PB2^xvi	3.993 (2)	P—O1	1.515 (6)
PB1—PB2^xvii	3.865 (10)	P—O1^i	1.515 (6)
PB1—PB2^xviii	3.865 (10)	P—O1^ii	1.515 (6)
PB1—PB2^xix	4.116 (10)	P—O1^li	3.461 (11)
PB1—PB2^xx	3.993 (2)	P—O1^lii	3.29 (2)
PB1—PB2^xxi	3.865 (10)	P—O1^liii	3.461 (11)
PB1—PB2^xxii	3.993 (2)	P—O1^liv	3.461 (11)
PB1—PB2^xxiii	4.116 (10)	P—O1^lv	3.461 (11)
PB1—PB2^xxiv	4.116 (10)	P—O1^lvi	3.29 (2)
PB1—PB2^xxv	3.865 (10)	P—O1^lvii	3.29 (2)
PB1—PB2^xxvi	3.993 (2)	P—O1^lviii	3.461 (11)
PB1—PB2^xxvii	3.993 (2)	P—O1^lix	3.461 (11)
PB1—PB2^xxviii	4.116 (10)	P—O2^lxxxv	4.230 (7)
PB1—PB2^xxix	3.865 (10)	P—O2	1.536 (4)
PB1—PB2^xxx	4.116 (10)	P—O2^lxxxvi	4.310 (7)
PB1—PB2^xxxi	3.865 (10)	P—O2^i	1.536 (4)
PB1—PB2^xxxii	3.993 (2)	P—O2^lxxxvii	4.310 (7)
PB1—PB2^xxxiii	3.865 (10)	P—O2^lxxxviii	4.230 (7)
PB1—PB2^xxxiv	3.993 (2)	P—O2^lxxxix	4.310 (7)
PB1—PB2^xxxv	4.116 (10)	P—O2^xc	4.230 (7)
PB1—PB2^xxxvi	3.993 (2)	P—O2^ii	1.536 (4)
PB1—PB2^xxxvii	4.116 (10)	P—O2^xci	4.230 (7)
PB1—PB2^xxxviii	3.865 (10)	P—O2^xcii	4.310 (7)
PB1—PB2^xxxix	4.116 (10)	P—O2^iii	1.536 (4)
PB1—PB2^xl	3.993 (2)	P—O2^xciii	4.310 (7)
PB1—PB2^xli	3.865 (10)	P—O2^iv	1.536 (4)
PB1—PB2^xlii	3.993 (2)	P—O2^xciv	4.230 (7)
PB1—PB2^xliii	3.865 (10)	P—O2^v	1.536 (4)
PB1—PB2^xliv	4.116 (10)	P—O2^xcv	4.230 (7)
PB1—PB2^xlv	3.865 (10)	P—O2^xcvi	4.310 (7)
PB1—PB2^xlvi	4.116 (10)	P—O2^lxxxiv	3.614 (7)
PB1—PB2^xlvii	3.993 (2)	P—O2^xcvii	3.614 (7)
PB1—P^xii	3.439 (2)	P—O2^xcviii	3.614 (7)
PB1—P^xiii	3.439 (2)	P—O2^xcix	3.614 (7)
PB1—P^xiv	3.439 (2)	P—O2^100	3.614 (7)
PB1—P^xxx	3.439 (2)	P—O2^101	3.614 (7)
PB1—P^xxxi	3.439 (2)	P—O2^li	4.354 (9)
PB1—P^xxxii	3.439 (2)	P—O2^liii	4.275 (8)
PB1—O1^xii	3.074 (10)	P—O2^liv	4.275 (8)
PB1—O1^xiii	3.26 (2)	P—O2^lv	4.354 (9)
PB1—O1^xiv	3.074 (10)	P—O2^lviii	4.275 (8)
PB1—O1^xv	3.074 (10)	P—O2^lix	4.354 (9)
PB1—O1^xvi	3.074 (10)	P—O2^lx	4.354 (9)
PB1—O1^xvii	3.26 (2)	P—O2^lxi	4.275 (8)
PB1—O1^xviii	3.26 (2)	P—O2^lxii	4.275 (8)
PB1—O1^xix	3.074 (10)	P—O2^lxiii	4.354 (9)
PB1—O1^xx	3.074 (10)	P—O2^lxiv	4.354 (9)
PB1—O1^xxx	3.074 (10)	P—O2^lxv	4.275 (8)
PB1—O1^xxxi	3.26 (2)	O1—PB1^xlviii	3.074 (10)
PB1—O1^xxxii	3.074 (10)	O1—PB1^xlix	3.26 (2)
PB1—O1^xxxiii	3.26 (2)	O1—PB1^l	3.074 (10)
PB1—O1^xxxiv	3.074 (10)	O1—PB2	2.393 (7)
PB1—O1^xxxv	3.074 (10)	O1—PB2^i	2.385 (7)
PB1—O1^xxxvi	3.074 (10)	O1—PB2^ii	2.377 (7)
PB1—O1^xxxvii	3.074 (10)	O1—PB2^iii	2.385 (7)
PB1—O1^xxxviii	3.26 (2)	O1—PB2^iv	2.393 (7)
PB1—O2^xiii	2.569 (4)	O1—PB2^v	2.377 (7)
PB1—O2^xvii	2.569 (4)	O1—PB2^li	4.096 (9)
PB1—O2^xviii	2.569 (4)	O1—PB2^lii	4.075 (19)
PB1—O2^xxi	2.569 (4)	O1—PB2^liii	3.972 (12)
PB1—O2^xxv	2.569 (4)	O1—PB2^liv	3.977 (13)
PB1—O2^xxix	2.569 (4)	O1—PB2^lv	3.955 (17)
PB1—O2^xxxi	2.569 (4)	O1—PB2^lvi	4.221 (15)
PB1—O2^xxxiii	2.569 (4)	O1—PB2^lvii	4.225 (15)
PB1—O2^xxxviii	2.569 (4)	O1—PB2^lviii	3.83 (2)
PB1—O2^xli	2.569 (4)	O1—PB2^lix	4.105 (11)
PB1—O2^xliii	2.569 (4)	O1—PB2^lxvi	4.221 (15)
PB1—O2^xlv	2.569 (4)	O1—PB2^lx	3.955 (17)
PB2—PB1	4.201 (4)	O1—PB2^lxi	3.977 (13)
PB2—PB1^xlviii	4.116 (10)	O1—PB2^lxii	3.972 (12)
PB2—PB1^xlix	3.865 (10)	O1—PB2^lxvii	4.075 (19)
PB2—PB1^l	3.993 (2)	O1—PB2^lxiii	4.096 (9)
PB2—PB2^i	0.32 (3)	O1—PB2^lxiv	4.105 (11)
PB2—PB2^ii	0.32 (3)	O1—PB2^lxv	3.83 (2)
PB2—PB2^iii	0.184 (14)	O1—PB2^lxviii	4.225 (15)
PB2—PB2^iv	0.184 (14)	O1—P	1.515 (6)
PB2—PB2^v	0.37 (3)	O1—P^li	3.461 (11)
PB2—PB2^xxx	3.87 (2)	O1—P^lii	3.29 (2)
PB2—PB2^xxxi	3.31 (2)	O1—P^liii	3.461 (11)
PB2—PB2^xxxii	3.598 (5)	O1—O1^i	0.22 (4)
PB2—PB2^xxxiii	3.584 (4)	O1—O1^ii	0.22 (4)
PB2—PB2^xxxiv	3.441 (11)	O1—O1^li	3.27 (2)
PB2—PB2^xxxv	3.721 (12)	O1—O1^lii	2.89 (4)
PB2—PB2^xxxvi	3.721 (12)	O1—O1^liii	3.27 (2)
PB2—PB2^xxxvii	3.584 (4)	O1—O1^liv	3.26 (2)
PB2—PB2^xxxviii	3.441 (11)	O1—O1^lv	3.079 (10)
PB2—PB2^xxxix	3.86 (2)	O1—O1^lvi	3.079 (10)
PB2—PB2^xl	3.451 (10)	O1—O1^lvii	3.079 (10)
PB2—PB2^xli	3.451 (10)	O1—O1^lviii	3.079 (10)
PB2—PB2^xlii	3.730 (13)	O1—O1^lix	3.26 (2)
PB2—PB2^xliii	3.30 (2)	O1—O2	2.565 (14)
PB2—PB2^xliv	3.730 (13)	O1—O2^i	2.460 (8)
PB2—PB2^xlv	3.579 (4)	O1—O2^ii	2.454 (8)
PB2—PB2^xlvi	3.579 (4)	O1—O2^iii	2.460 (8)
PB2—PB2^xlvii	3.579 (4)	O1—O2^iv	2.565 (14)
PB2—P	3.889 (8)	O1—O2^v	2.454 (8)
PB2—P^xii	4.193 (5)	O1—O2^li	3.341 (10)
PB2—P^xiii	4.311 (10)	O1—O2^liii	3.237 (9)
PB2—P^xiv	4.072 (11)	O1—O2^liv	3.318 (17)
PB2—P^li	3.3100 (19)	O1—O2^lv	3.243 (17)
PB2—P^lii	3.458 (12)	O1—O2^lviii	3.141 (19)
PB2—P^liii	3.155 (12)	O1—O2^lix	3.42 (2)
PB2—O1	2.393 (7)	O1—O2^lx	3.243 (17)
PB2—O1^i	2.377 (7)	O1—O2^lxi	3.318 (17)
PB2—O1^ii	2.385 (7)	O1—O2^lxii	3.237 (9)
PB2—O1^li	4.096 (9)	O1—O2^lxiii	3.341 (10)
PB2—O1^lii	4.075 (19)	O1—O2^lxiv	3.42 (2)
PB2—O1^liii	3.972 (12)	O1—O2^lxv	3.141 (19)
PB2—O1^liv	4.105 (11)	O2—PB1^xlix	2.569 (4)
PB2—O1^lv	4.225 (15)	O2—PB2^li	2.918 (13)
PB2—O1^lvi	3.83 (2)	O2—PB2^liii	2.614 (12)
PB2—O1^lvii	3.955 (17)	O2—PB2^liv	2.649 (17)
PB2—O1^lviii	4.221 (15)	O2—PB2^lvi	2.888 (17)
PB2—O1^lix	3.977 (13)	O2—PB2^lvii	2.931 (13)
PB2—O2^xiii	2.922 (8)	O2—PB2^lix	2.629 (12)
PB2—O2^xvii	2.731 (9)	O2—PB2^lxvi	3.011 (17)
PB2—O2^xviii	2.834 (4)	O2—PB2^lxi	2.526 (18)
PB2—O2^xxi	2.826 (4)	O2—PB2^lxii	2.737 (12)
PB2—O2^xxv	2.926 (8)	O2—PB2^lxiii	2.795 (12)
PB2—O2^xxix	2.735 (9)	O2—PB2^lxiv	2.751 (12)
PB2—O2^li	2.918 (13)	O2—PB2^lxviii	2.809 (13)
PB2—O2^liii	2.614 (12)	O2—PB2^xlix	2.922 (8)
PB2—O2^liv	2.629 (12)	O2—PB2^lxx	2.834 (4)
PB2—O2^lv	2.931 (13)	O2—PB2^lxxiii	2.731 (9)
PB2—O2^lviii	2.888 (17)	O2—PB2^lxxvi	2.826 (4)
PB2—O2^lix	2.649 (17)	O2—PB2^lxxix	2.926 (8)
PB2—O2^lx	3.011 (17)	O2—PB2^lxxxii	2.735 (9)
PB2—O2^lxi	2.526 (18)	O2—P^102	4.310 (7)
PB2—O2^lxii	2.795 (12)	O2—P	1.536 (4)
PB2—O2^lxiii	2.737 (12)	O2—P^103	4.230 (7)
PB2—O2^lxiv	2.751 (12)	O2—P^lxxxiv	3.614 (7)
PB2—O2^lxv	2.809 (13)	O2—P^li	4.354 (9)
P—PB1^xlviii	3.439 (2)	O2—P^liii	4.275 (8)
P—PB1^xlix	3.439 (2)	O2—O1	2.565 (14)
P—PB1^l	3.439 (2)	O2—O1^i	2.454 (8)
P—PB2	3.889 (8)	O2—O1^ii	2.460 (8)
P—PB2^i	3.889 (8)	O2—O1^li	3.341 (10)
P—PB2^ii	3.889 (8)	O2—O1^liii	3.237 (9)
P—PB2^iii	3.889 (8)	O2—O1^liv	3.42 (2)
P—PB2^iv	3.889 (8)	O2—O1^lvi	3.141 (19)
P—PB2^v	3.889 (8)	O2—O1^lvii	3.243 (17)
P—PB2^li	3.3100 (19)	O2—O1^lix	3.318 (17)
P—PB2^lii	3.458 (12)	O2—O2^i	2.504 (6)
P—PB2^liii	3.155 (12)	O2—O2^lxxxvii	2.927 (7)
P—PB2^liv	3.155 (12)	O2—O2^xc	2.927 (7)
P—PB2^lv	3.3100 (19)	O2—O2^ii	2.504 (6)
P—PB2^lvi	3.458 (12)	O2—O2^xcii	2.988 (12)
P—PB2^lvii	3.458 (12)	O2—O2^iii	2.439 (12)
P—PB2^lviii	3.155 (12)	O2—O2^iv	0.13 (2)
P—PB2^lix	3.3100 (19)	O2—O2^v	2.565 (12)
P—PB2^lxvi	3.458 (12)	O2—O2^xcv	2.863 (12)
P—PB2^lx	3.3100 (19)	O2—O2^104	4.376 (15)
P—PB2^lxi	3.155 (12)	O2—O2^lxxxiv	4.022 (7)
P—PB2^lxii	3.155 (12)	O2—O2^105	4.218 (14)
P—PB2^lxvii	3.458 (12)	O2—O2^xcvii	3.147 (7)
P—PB2^lxiii	3.3100 (19)	O2—O2^xcviii	3.147 (7)
P—PB2^lxiv	3.3100 (19)	O2—O2^xcix	3.197 (11)
P—PB2^lxv	3.155 (12)	O2—O2^106	4.296 (5)
P—PB2^lxviii	3.458 (12)	O2—O2^100	4.020 (7)
P—PB2^xlviii	4.072 (11)	O2—O2^107	4.296 (5)
P—PB2^xlix	4.311 (10)	O2—O2^101	3.098 (10)
P—PB2^l	4.193 (5)	O2—O2^liv	4.223 (7)
P—PB2^lxix	4.311 (10)	O2—O2^lix	4.223 (7)
P—PB2^lxx	4.193 (5)	O2—O2^lxi	4.180 (9)
P—PB2^lxxi	4.072 (11)	O2—O2^lxiv	4.267 (10)
PB2^i—PB2—PB2^ii	60.0	O1^ii—P—O2	107.5 (5)
PB2^i—PB2—PB2^iii	90.0000 (2)	O1^ii—P—O2^i	107.1 (5)
PB2^i—PB2—PB2^iv	30.0000 (9)	O1^ii—P—O2^ii	114.4 (9)
PB2^i—PB2—PB2^v	30.0	O1^ii—P—O2^iii	114.4 (9)
PB2^ii—PB2—PB2^iii	30.0000 (9)	O1^ii—P—O2^iv	107.1 (5)
PB2^ii—PB2—PB2^iv	90.0000 (2)	O1^ii—P—O2^v	107.5 (5)
PB2^ii—PB2—PB2^v	30.0	O2—P—O2^i	109.2 (2)
PB2^iii—PB2—PB2^iv	120.0000 (19)	O2—P—O2^ii	109.2 (2)
PB2^iii—PB2—PB2^v	60.0000 (4)	O2—P—O2^iii	105.1 (7)
PB2^iv—PB2—PB2^v	60.0000 (4)	O2—P—O2^iv	4.7 (8)
O1—P—O1^i	8.2 (14)	O2—P—O2^v	113.2 (7)
O1—P—O1^ii	8.2 (14)	O2^i—P—O2^ii	109.2 (2)
O1—P—O2	114.4 (9)	O2^i—P—O2^iii	113.2 (7)
O1—P—O2^i	107.5 (5)	O2^i—P—O2^iv	105.1 (7)
O1—P—O2^ii	107.1 (5)	O2^i—P—O2^v	4.7 (8)
O1—P—O2^iii	107.5 (5)	O2^ii—P—O2^iii	4.7 (8)
O1—P—O2^iv	114.4 (9)	O2^ii—P—O2^iv	113.2 (7)
O1—P—O2^v	107.1 (5)	O2^ii—P—O2^v	105.1 (7)
O1^i—P—O1^ii	8.2 (14)	O2^iii—P—O2^iv	109.2 (2)
O1^i—P—O2	107.1 (5)	O2^iii—P—O2^v	109.2 (2)
O1^i—P—O2^i	114.4 (9)	O2^iv—P—O2^v	109.2 (2)
O1^i—P—O2^ii	107.5 (5)	P—O1—O1^i	85.9 (7)
O1^i—P—O2^iii	107.1 (5)	P—O1—O1^ii	85.9 (7)
O1^i—P—O2^iv	107.5 (5)	O1^i—O1—O1^ii	60.0
O1^i—P—O2^v	114.4 (9)	P—O2—O2^iv	87.7 (4)

Symmetry codes: (i) z, x, y; (ii) y, z, x; (iii) x, y, −z; (iv) −z, x, y; (v) y, −z, x; (vi) −x, −y, −z; (vii) −z, −x, −y; (viii) −y, −z, −x; (ix) −x, −y, z; (x) z, −x, −y; (xi) −y, z, −x; (xii) x−1, y−1/2, z−1/2; (xiii) x, y−1/2, z−1/2; (xiv) x, y+1/2, z−1/2; (xv) z−1, x−1/2, y−1/2; (xvi) z, x−1/2, y−1/2; (xvii) z, x+1/2, y−1/2; (xviii) y−1, z−1/2, x−1/2; (xix) y, z−1/2, x−1/2; (xx) y, z+1/2, x−1/2; (xxi) x−1, y−1/2, −z−1/2; (xxii) x, y−1/2, −z−1/2; (xxiii) x, y+1/2, −z−1/2; (xxiv) −z−1, x−1/2, y−1/2; (xxv) −z, x−1/2, y−1/2; (xxvi) −z, x+1/2, y−1/2; (xxvii) y−1, −z−1/2, x−1/2; (xxviii) y, −z−1/2, x−1/2; (xxix) y, −z+1/2, x−1/2; (xxx) −x−1/2, −y−1, −z+1/2; (xxxi) −x−1/2, −y, −z+1/2; (xxxii) −x+1/2, −y, −z+1/2; (xxxiii) −z−1/2, −x−1, −y+1/2; (xxxiv) −z−1/2, −x, −y+1/2; (xxxv) −z+1/2, −x, −y+1/2; (xxxvi) −y−1/2, −z−1, −x+1/2; (xxxvii) −y−1/2, −z, −x+1/2; (xxxviii) −y+1/2, −z, −x+1/2; (xxxix) −x−1/2, −y−1, z+1/2; (xl) −x−1/2, −y, z+1/2; (xli) −x+1/2, −y, z+1/2; (xlii) z−1/2, −x−1, −y+1/2; (xliii) z−1/2, −x, −y+1/2; (xliv) z+1/2, −x, −y+1/2; (xlv) −y−1/2, z−1, −x+1/2; (xlvi) −y−1/2, z, −x+1/2; (xlvii) −y+1/2, z, −x+1/2; (xlviii) x−1/2, y−1, z+1/2; (xlix) x−1/2, y, z+1/2; (l) x+1/2, y, z+1/2; (li) −x−1, −y−1/2, −z+1/2; (lii) −x, −y−1/2, −z+1/2; (liii) −x, −y+1/2, −z+1/2; (liv) −z−1, −x−1/2, −y+1/2; (lv) −z, −x−1/2, −y+1/2; (lvi) −z, −x+1/2, −y+1/2; (lvii) −y−1, −z−1/2, −x+1/2; (lviii) −y, −z−1/2, −x+1/2; (lix) −y, −z+1/2, −x+1/2; (lx) −x, −y−1/2, z+1/2; (lxi) −x, −y+1/2, z+1/2; (lxii) z−1, −x−1/2, −y+1/2; (lxiii) z, −x+1/2, −y+1/2; (lxiv) −y−1, z−1/2, −x+1/2; (lxv) −y, z−1/2, −x+1/2; (lxvi) −x−1, −y−1/2, z+1/2; (lxvii) z, −x−1/2, −y+1/2; (lxviii) −y, z+1/2, −x+1/2; (lxix) z−1/2, x−1, y+1/2; (lxx) z−1/2, x, y+1/2; (lxxi) z+1/2, x, y+1/2; (lxxii) y−1/2, z−1, x+1/2; (lxxiii) y−1/2, z, x+1/2; (lxxiv) y+1/2, z, x+1/2; (lxxv) x−1/2, y−1, −z+1/2; (lxxvi) x−1/2, y, −z+1/2; (lxxvii) x+1/2, y, −z+1/2; (lxxviii) −z−1/2, x−1, y+1/2; (lxxix) −z−1/2, x, y+1/2; (lxxx) −z+1/2, x, y+1/2; (lxxxi) y−1/2, −z−1, x+1/2; (lxxxii) y−1/2, −z, x+1/2; (lxxxiii) y+1/2, −z, x+1/2; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) z, x+1, y; (lxxxviii) z+1, x+1, y; (lxxxix) y−1, z−1, x; (xc) y−1, z, x; (xci) x−1, y−1, −z; (xcii) x−1, y, −z; (xciii) −z, x−1, y; (xciv) −z+1, x, y; (xcv) y, −z+1, x; (xcvi) y+1, −z+1, x; (xcvii) −z, −x, −y+1; (xcviii) −y, −z, −x+1; (xcix) −x, −y, z+1; (100) z, −x, −y+1; (101) −y, z, −x+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x−1, −y, −z+1; (105) −x, −y+1, −z+1; (106) z−1, −x, −y+1; (107) z, −x+1, −y+1.

(S4P43_phase_1)

Crystal data

O8.00P2Pb3.00	Z = 3
Mr = 811.54	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.4368 (2) Å	Particle morphology: plate
c = 20.0175 (10) Å	irregular, 6 × 6 mm
V = 512.42 (4) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.031	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 76.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 8.32 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 132.1 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 247.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.029	37 parameters
Rexp = 0.015	9 restraints
R(F^2) = 0.17705	(Δ/σ)max = 0.06
χ^2 = 4.000	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 3.51608 2: -1.00996 3: 1.62909 4: -0.377363 5: 0.687305 6: -0.296244 7: 0.392229 8: -0.165049 9: 0.194674 10: -0.106028 11: 8.209180E-0212: -9.164950E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.91437 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
PB1	0.0	0.0	0.0	0.0196 (14)*
PB2	0.0	0.033 (2)	0.21003 (15)	0.0196 (14)*	0.16667
P	0.0	0.0	0.4039 (3)	0.0109 (12)*
O1	0.0141 (17)	−0.0141 (17)	0.3283 (2)	0.0158 (10)*	0.3333
O2	−0.144 (3)	0.164 (3)	0.42980 (13)	0.0158 (10)*	0.5

Geometric parameters (Å, º)

PB1—PB2	4.208 (3)	P—PB2^lxxii	4.204 (4)
PB1—PB2^i	4.208 (3)	P—PB2^lxxiii	4.088 (10)
PB1—PB2^ii	4.208 (3)	P—PB2^lxxiv	4.318 (9)
PB1—PB2^iii	4.208 (3)	P—PB2^lxxv	4.088 (10)
PB1—PB2^iv	4.208 (3)	P—PB2^lxxvi	4.204 (4)
PB1—PB2^v	4.208 (3)	P—PB2^lxxvii	4.318 (9)
PB1—PB2^vi	4.208 (3)	P—PB2^lxxviii	4.204 (4)
PB1—PB2^vii	4.208 (3)	P—PB2^lxxix	4.318 (9)
PB1—PB2^viii	4.208 (3)	P—PB2^lxxx	4.088 (10)
PB1—PB2^ix	4.208 (3)	P—PB2^lxxxi	4.318 (9)
PB1—PB2^x	4.208 (3)	P—PB2^lxxxii	4.088 (10)
PB1—PB2^xi	4.208 (3)	P—PB2^lxxxiii	4.204 (4)
PB1—PB2^xii	3.9971 (19)	P—P^lxxxiv	3.847 (11)
PB1—PB2^xiii	3.874 (8)	P—P^li	4.223 (7)
PB1—PB2^xiv	4.116 (9)	P—P^lii	4.223 (7)
PB1—PB2^xv	4.116 (9)	P—P^liii	4.223 (7)
PB1—PB2^xvi	3.9971 (19)	P—O1	1.519 (7)
PB1—PB2^xvii	3.874 (8)	P—O1^i	1.519 (7)
PB1—PB2^xviii	3.874 (8)	P—O1^ii	1.519 (7)
PB1—PB2^xix	4.116 (9)	P—O1^li	3.465 (9)
PB1—PB2^xx	3.9971 (19)	P—O1^lii	3.280 (15)
PB1—PB2^xxi	3.874 (8)	P—O1^liii	3.465 (9)
PB1—PB2^xxii	3.9971 (19)	P—O1^liv	3.465 (9)
PB1—PB2^xxiii	4.116 (9)	P—O1^lv	3.465 (9)
PB1—PB2^xxiv	4.116 (9)	P—O1^lvi	3.280 (15)
PB1—PB2^xxv	3.874 (8)	P—O1^lvii	3.280 (15)
PB1—PB2^xxvi	3.9971 (19)	P—O1^lviii	3.465 (9)
PB1—PB2^xxvii	3.9971 (19)	P—O1^lix	3.465 (9)
PB1—PB2^xxviii	4.116 (9)	P—O2^lxxxv	4.243 (9)
PB1—PB2^xxix	3.874 (8)	P—O2	1.540 (4)
PB1—PB2^xxx	4.116 (9)	P—O2^lxxxvi	4.309 (9)
PB1—PB2^xxxi	3.874 (8)	P—O2^i	1.540 (4)
PB1—PB2^xxxii	3.9971 (19)	P—O2^lxxxvii	4.309 (9)
PB1—PB2^xxxiii	3.874 (8)	P—O2^lxxxviii	4.243 (9)
PB1—PB2^xxxiv	3.9971 (19)	P—O2^lxxxix	4.309 (9)
PB1—PB2^xxxv	4.116 (9)	P—O2^xc	4.243 (9)
PB1—PB2^xxxvi	3.9971 (19)	P—O2^ii	1.540 (4)
PB1—PB2^xxxvii	4.116 (9)	P—O2^xci	4.243 (9)
PB1—PB2^xxxviii	3.874 (8)	P—O2^xcii	4.309 (9)
PB1—PB2^xxxix	4.116 (9)	P—O2^iii	1.540 (4)
PB1—PB2^xl	3.9971 (19)	P—O2^xciii	4.309 (9)
PB1—PB2^xli	3.874 (8)	P—O2^iv	1.540 (4)
PB1—PB2^xlii	3.9971 (19)	P—O2^xciv	4.243 (9)
PB1—PB2^xliii	3.874 (8)	P—O2^v	1.540 (4)
PB1—PB2^xliv	4.116 (9)	P—O2^xcv	4.243 (9)
PB1—PB2^xlv	3.874 (8)	P—O2^xcvi	4.309 (9)
PB1—PB2^xlvi	4.116 (9)	P—O2^lxxxiv	3.631 (6)
PB1—PB2^xlvii	3.9971 (19)	P—O2^xcvii	3.631 (6)
PB1—P^xii	3.442 (2)	P—O2^xcviii	3.631 (6)
PB1—P^xiii	3.442 (2)	P—O2^xcix	3.631 (6)
PB1—P^xiv	3.442 (2)	P—O2^100	3.631 (6)
PB1—P^xxx	3.442 (2)	P—O2^101	3.631 (6)
PB1—P^xxxi	3.442 (2)	P—O2^li	4.344 (10)
PB1—P^xxxii	3.442 (2)	P—O2^liii	4.278 (9)
PB1—O1^xii	3.076 (8)	P—O2^liv	4.278 (9)
PB1—O1^xiii	3.273 (16)	P—O2^lv	4.344 (10)
PB1—O1^xiv	3.076 (8)	P—O2^lviii	4.278 (9)
PB1—O1^xv	3.076 (8)	P—O2^lix	4.344 (10)
PB1—O1^xvi	3.076 (8)	P—O2^lx	4.344 (10)
PB1—O1^xvii	3.273 (16)	P—O2^lxi	4.278 (9)
PB1—O1^xviii	3.273 (16)	P—O2^lxii	4.278 (9)
PB1—O1^xix	3.076 (8)	P—O2^lxiii	4.344 (10)
PB1—O1^xx	3.076 (8)	P—O2^lxiv	4.344 (10)
PB1—O1^xxx	3.076 (8)	P—O2^lxv	4.278 (9)
PB1—O1^xxxi	3.273 (16)	O1—PB1^xlviii	3.076 (8)
PB1—O1^xxxii	3.076 (8)	O1—PB1^xlix	3.273 (16)
PB1—O1^xxxiii	3.273 (16)	O1—PB1^l	3.076 (8)
PB1—O1^xxxiv	3.076 (8)	O1—PB2	2.387 (6)
PB1—O1^xxxv	3.076 (8)	O1—PB2^i	2.378 (5)
PB1—O1^xxxvi	3.076 (8)	O1—PB2^ii	2.369 (5)
PB1—O1^xxxvii	3.076 (8)	O1—PB2^iii	2.378 (5)
PB1—O1^xxxviii	3.273 (16)	O1—PB2^iv	2.387 (6)
PB1—O2^xiii	2.566 (3)	O1—PB2^v	2.369 (5)
PB1—O2^xvii	2.566 (3)	O1—PB2^li	4.108 (7)
PB1—O2^xviii	2.566 (3)	O1—PB2^lii	4.074 (15)
PB1—O2^xxi	2.566 (3)	O1—PB2^liii	3.989 (10)
PB1—O2^xxv	2.566 (3)	O1—PB2^liv	3.994 (10)
PB1—O2^xxix	2.566 (3)	O1—PB2^lv	3.958 (13)
PB1—O2^xxxi	2.566 (3)	O1—PB2^lvi	4.229 (12)
PB1—O2^xxxiii	2.566 (3)	O1—PB2^lvii	4.234 (13)
PB1—O2^xxxviii	2.566 (3)	O1—PB2^lviii	3.839 (15)
PB1—O2^xli	2.566 (3)	O1—PB2^lix	4.118 (8)
PB1—O2^xliii	2.566 (3)	O1—PB2^lxvi	4.229 (12)
PB1—O2^xlv	2.566 (3)	O1—PB2^lx	3.958 (13)
PB2—PB1	4.208 (3)	O1—PB2^lxi	3.994 (10)
PB2—PB1^xlviii	4.116 (9)	O1—PB2^lxii	3.989 (10)
PB2—PB1^xlix	3.874 (8)	O1—PB2^lxvii	4.074 (15)
PB2—PB1^l	3.9971 (19)	O1—PB2^lxiii	4.108 (7)
PB2—PB2^i	0.31 (2)	O1—PB2^lxiv	4.118 (8)
PB2—PB2^ii	0.31 (2)	O1—PB2^lxv	3.839 (15)
PB2—PB2^iii	0.178 (12)	O1—PB2^lxviii	4.234 (13)
PB2—PB2^iv	0.178 (12)	O1—P	1.519 (7)
PB2—PB2^v	0.36 (3)	O1—P^li	3.465 (9)
PB2—PB2^xxx	3.86 (2)	O1—P^lii	3.280 (15)
PB2—PB2^xxxi	3.326 (18)	O1—P^liii	3.465 (9)
PB2—PB2^xxxii	3.605 (4)	O1—O1^i	0.23 (3)
PB2—PB2^xxxiii	3.591 (3)	O1—O1^ii	0.23 (3)
PB2—PB2^xxxiv	3.454 (9)	O1—O1^li	3.286 (18)
PB2—PB2^xxxv	3.724 (10)	O1—O1^lii	2.88 (3)
PB2—PB2^xxxvi	3.724 (10)	O1—O1^liii	3.286 (18)
PB2—PB2^xxxvii	3.591 (3)	O1—O1^liv	3.278 (16)
PB2—PB2^xxxviii	3.454 (9)	O1—O1^lv	3.081 (8)
PB2—PB2^xxxix	3.859 (19)	O1—O1^lvi	3.081 (8)
PB2—PB2^xl	3.463 (8)	O1—O1^lvii	3.081 (8)
PB2—PB2^xli	3.463 (8)	O1—O1^lviii	3.081 (8)
PB2—PB2^xlii	3.732 (11)	O1—O1^lix	3.278 (16)
PB2—PB2^xliii	3.321 (18)	O1—O2	2.575 (11)
PB2—PB2^xliv	3.732 (11)	O1—O2^i	2.463 (6)
PB2—PB2^xlv	3.587 (3)	O1—O2^ii	2.458 (7)
PB2—PB2^xlvi	3.587 (3)	O1—O2^iii	2.463 (6)
PB2—PB2^xlvii	3.587 (3)	O1—O2^iv	2.575 (11)
PB2—P	3.885 (7)	O1—O2^v	2.458 (7)
PB2—P^xii	4.204 (4)	O1—O2^li	3.330 (12)
PB2—P^xiii	4.318 (9)	O1—O2^liii	3.244 (11)
PB2—P^xiv	4.088 (10)	O1—O2^liv	3.330 (15)
PB2—P^li	3.3164 (17)	O1—O2^lv	3.226 (14)
PB2—P^lii	3.459 (10)	O1—O2^lviii	3.140 (18)
PB2—P^liii	3.167 (11)	O1—O2^lix	3.417 (18)
PB2—O1	2.387 (6)	O1—O2^lx	3.226 (14)
PB2—O1^i	2.369 (5)	O1—O2^lxi	3.330 (15)
PB2—O1^ii	2.378 (5)	O1—O2^lxii	3.244 (11)
PB2—O1^li	4.108 (7)	O1—O2^lxiii	3.330 (12)
PB2—O1^lii	4.074 (15)	O1—O2^lxiv	3.417 (18)
PB2—O1^liii	3.989 (10)	O1—O2^lxv	3.140 (18)
PB2—O1^liv	4.118 (8)	O2—PB1^xlix	2.566 (3)
PB2—O1^lv	4.234 (13)	O2—PB2^li	2.910 (15)
PB2—O1^lvi	3.839 (15)	O2—PB2^liii	2.633 (15)
PB2—O1^lvii	3.958 (13)	O2—PB2^liv	2.650 (18)
PB2—O1^lviii	4.229 (12)	O2—PB2^lvi	2.897 (17)
PB2—O1^lix	3.994 (10)	O2—PB2^lvii	2.922 (15)
PB2—O2^xiii	2.927 (7)	O2—PB2^lix	2.647 (14)
PB2—O2^xvii	2.744 (8)	O2—PB2^lxvi	2.999 (18)
PB2—O2^xviii	2.842 (4)	O2—PB2^lxi	2.549 (18)
PB2—O2^xxi	2.835 (4)	O2—PB2^lxii	2.735 (14)
PB2—O2^xxv	2.930 (7)	O2—PB2^lxiii	2.807 (14)
PB2—O2^xxix	2.747 (8)	O2—PB2^lxiv	2.748 (14)
PB2—O2^li	2.910 (15)	O2—PB2^lxviii	2.821 (14)
PB2—O2^liii	2.633 (15)	O2—PB2^xlix	2.927 (7)
PB2—O2^liv	2.647 (14)	O2—PB2^lxx	2.842 (4)
PB2—O2^lv	2.922 (15)	O2—PB2^lxxiii	2.744 (8)
PB2—O2^lviii	2.897 (17)	O2—PB2^lxxvi	2.835 (4)
PB2—O2^lix	2.650 (18)	O2—PB2^lxxix	2.930 (7)
PB2—O2^lx	2.999 (18)	O2—PB2^lxxxii	2.747 (8)
PB2—O2^lxi	2.549 (18)	O2—P^102	4.309 (9)
PB2—O2^lxii	2.807 (14)	O2—P	1.540 (4)
PB2—O2^lxiii	2.735 (14)	O2—P^103	4.243 (9)
PB2—O2^lxiv	2.748 (14)	O2—P^lxxxiv	3.631 (6)
PB2—O2^lxv	2.821 (14)	O2—P^li	4.344 (10)
P—PB1^xlviii	3.442 (2)	O2—P^liii	4.278 (9)
P—PB1^xlix	3.442 (2)	O2—O1	2.575 (11)
P—PB1^l	3.442 (2)	O2—O1^i	2.458 (7)
P—PB2	3.885 (7)	O2—O1^ii	2.463 (6)
P—PB2^i	3.885 (7)	O2—O1^li	3.330 (12)
P—PB2^ii	3.885 (7)	O2—O1^liii	3.244 (11)
P—PB2^iii	3.885 (7)	O2—O1^liv	3.417 (18)
P—PB2^iv	3.885 (7)	O2—O1^lvi	3.140 (18)
P—PB2^v	3.885 (7)	O2—O1^lvii	3.226 (14)
P—PB2^li	3.3164 (17)	O2—O1^lix	3.330 (15)
P—PB2^lii	3.459 (10)	O2—O2^i	2.512 (6)
P—PB2^liii	3.167 (11)	O2—O2^lxxxvii	2.928 (6)
P—PB2^liv	3.167 (11)	O2—O2^xc	2.928 (6)
P—PB2^lv	3.3164 (17)	O2—O2^ii	2.512 (6)
P—PB2^lvi	3.459 (10)	O2—O2^xcii	2.979 (15)
P—PB2^lvii	3.459 (10)	O2—O2^iii	2.458 (15)
P—PB2^lviii	3.167 (11)	O2—O2^iv	0.10 (3)
P—PB2^lix	3.3164 (17)	O2—O2^v	2.562 (14)
P—PB2^lxvi	3.459 (10)	O2—O2^xcv	2.875 (14)
P—PB2^lx	3.3164 (17)	O2—O2^104	4.375 (18)
P—PB2^lxi	3.167 (11)	O2—O2^lxxxiv	4.039 (6)
P—PB2^lxii	3.167 (11)	O2—O2^105	4.244 (17)
P—PB2^lxvii	3.459 (10)	O2—O2^xcvii	3.163 (5)
P—PB2^lxiii	3.3164 (17)	O2—O2^xcviii	3.163 (5)
P—PB2^lxiv	3.3164 (17)	O2—O2^xcix	3.204 (12)
P—PB2^lxv	3.167 (11)	O2—O2^106	4.309 (4)
P—PB2^lxviii	3.459 (10)	O2—O2^100	4.037 (6)
P—PB2^xlviii	4.088 (10)	O2—O2^107	4.309 (4)
P—PB2^xlix	4.318 (9)	O2—O2^101	3.122 (11)
P—PB2^l	4.204 (4)	O2—O2^liv	4.216 (5)
P—PB2^lxix	4.318 (9)	O2—O2^lix	4.216 (5)
P—PB2^lxx	4.204 (4)	O2—O2^lxi	4.180 (10)
P—PB2^lxxi	4.088 (10)	O2—O2^lxiv	4.252 (11)
PB2^i—PB2—PB2^ii	60.0	O1^ii—P—O2	107.3 (4)
PB2^i—PB2—PB2^iii	90.0	O1^ii—P—O2^i	106.9 (4)
PB2^i—PB2—PB2^iv	30.0000 (9)	O1^ii—P—O2^ii	114.7 (6)
PB2^i—PB2—PB2^v	30.0	O1^ii—P—O2^iii	114.7 (6)
PB2^ii—PB2—PB2^iii	30.0000 (9)	O1^ii—P—O2^iv	106.9 (4)
PB2^ii—PB2—PB2^iv	90.0	O1^ii—P—O2^v	107.3 (4)
PB2^ii—PB2—PB2^v	30.0	O2—P—O2^i	109.3 (2)
PB2^iii—PB2—PB2^iv	120.0000 (13)	O2—P—O2^ii	109.3 (2)
PB2^iii—PB2—PB2^v	60.0000 (5)	O2—P—O2^iii	105.9 (9)
PB2^iv—PB2—PB2^v	60.0000 (5)	O2—P—O2^iv	3.9 (10)
O1—P—O1^i	8.7 (11)	O2—P—O2^v	112.6 (9)
O1—P—O1^ii	8.7 (11)	O2^i—P—O2^ii	109.3 (2)
O1—P—O2	114.7 (6)	O2^i—P—O2^iii	112.6 (9)
O1—P—O2^i	107.3 (4)	O2^i—P—O2^iv	105.9 (9)
O1—P—O2^ii	106.9 (4)	O2^i—P—O2^v	3.9 (10)
O1—P—O2^iii	107.3 (4)	O2^ii—P—O2^iii	3.9 (10)
O1—P—O2^iv	114.7 (6)	O2^ii—P—O2^iv	112.6 (9)
O1—P—O2^v	106.9 (4)	O2^ii—P—O2^v	105.9 (9)
O1^i—P—O1^ii	8.7 (11)	O2^iii—P—O2^iv	109.3 (2)
O1^i—P—O2	106.9 (4)	O2^iii—P—O2^v	109.3 (2)
O1^i—P—O2^i	114.7 (6)	O2^iv—P—O2^v	109.3 (2)
O1^i—P—O2^ii	107.3 (4)	P—O1—O1^i	85.7 (5)
O1^i—P—O2^iii	106.9 (4)	P—O1—O1^ii	85.7 (5)
O1^i—P—O2^iv	107.3 (4)	O1^i—O1—O1^ii	60.0
O1^i—P—O2^v	114.7 (6)	P—O2—O2^iv	88.1 (5)

Symmetry codes: (i) −y, x−y, z; (ii) y−x, −x, z; (iii) y−x, y, z; (iv) −y, −x, z; (v) x, x−y, z; (vi) −x, −y, −z; (vii) y, y−x, −z; (viii) x−y, x, −z; (ix) x−y, −y, −z; (x) y, x, −z; (xi) −x, y−x, −z; (xii) x−2/3, y−1/3, z−1/3; (xiii) x+1/3, y−1/3, z−1/3; (xiv) x+1/3, y+2/3, z−1/3; (xv) −y−2/3, x−y−1/3, z−1/3; (xvi) −y+1/3, x−y−1/3, z−1/3; (xvii) −y+1/3, x−y+2/3, z−1/3; (xviii) y−x−2/3, −x−1/3, z−1/3; (xix) y−x+1/3, −x−1/3, z−1/3; (xx) y−x+1/3, −x+2/3, z−1/3; (xxi) y−x−2/3, y−1/3, z−1/3; (xxii) y−x+1/3, y−1/3, z−1/3; (xxiii) y−x+1/3, y+2/3, z−1/3; (xxiv) −y−2/3, −x−1/3, z−1/3; (xxv) −y+1/3, −x−1/3, z−1/3; (xxvi) −y+1/3, −x+2/3, z−1/3; (xxvii) x−2/3, x−y−1/3, z−1/3; (xxviii) x+1/3, x−y−1/3, z−1/3; (xxix) x+1/3, x−y+2/3, z−1/3; (xxx) −x−2/3, −y−1/3, −z+2/3; (xxxi) −x−2/3, −y+2/3, −z+2/3; (xxxii) −x+1/3, −y+2/3, −z+2/3; (xxxiii) y−2/3, y−x−1/3, −z+2/3; (xxxiv) y−2/3, y−x+2/3, −z+2/3; (xxxv) y+1/3, y−x+2/3, −z+2/3; (xxxvi) x−y−2/3, x−1/3, −z+2/3; (xxxvii) x−y−2/3, x+2/3, −z+2/3; (xxxviii) x−y+1/3, x+2/3, −z+2/3; (xxxix) x−y−2/3, −y−1/3, −z+2/3; (xl) x−y−2/3, −y+2/3, −z+2/3; (xli) x−y+1/3, −y+2/3, −z+2/3; (xlii) y−2/3, x−1/3, −z+2/3; (xliii) y−2/3, x+2/3, −z+2/3; (xliv) y+1/3, x+2/3, −z+2/3; (xlv) −x−2/3, y−x−1/3, −z+2/3; (xlvi) −x−2/3, y−x+2/3, −z+2/3; (xlvii) −x+1/3, y−x+2/3, −z+2/3; (xlviii) x−1/3, y−2/3, z+1/3; (xlix) x−1/3, y+1/3, z+1/3; (l) x+2/3, y+1/3, z+1/3; (li) −x−1/3, −y−2/3, −z+1/3; (lii) −x+2/3, −y−2/3, −z+1/3; (liii) −x+2/3, −y+1/3, −z+1/3; (liv) y−1/3, y−x−2/3, −z+1/3; (lv) y+2/3, y−x−2/3, −z+1/3; (lvi) y+2/3, y−x+1/3, −z+1/3; (lvii) x−y−1/3, x−2/3, −z+1/3; (lviii) x−y+2/3, x−2/3, −z+1/3; (lix) x−y+2/3, x+1/3, −z+1/3; (lx) x−y+2/3, −y−2/3, −z+1/3; (lxi) x−y+2/3, −y+1/3, −z+1/3; (lxii) y−1/3, x−2/3, −z+1/3; (lxiii) y+2/3, x+1/3, −z+1/3; (lxiv) −x−1/3, y−x−2/3, −z+1/3; (lxv) −x+2/3, y−x−2/3, −z+1/3; (lxvi) x−y−1/3, −y−2/3, −z+1/3; (lxvii) y+2/3, x−2/3, −z+1/3; (lxviii) −x+2/3, y−x+1/3, −z+1/3; (lxix) −y−1/3, x−y−2/3, z+1/3; (lxx) −y−1/3, x−y+1/3, z+1/3; (lxxi) −y+2/3, x−y+1/3, z+1/3; (lxxii) y−x−1/3, −x−2/3, z+1/3; (lxxiii) y−x−1/3, −x+1/3, z+1/3; (lxxiv) y−x+2/3, −x+1/3, z+1/3; (lxxv) y−x−1/3, y−2/3, z+1/3; (lxxvi) y−x−1/3, y+1/3, z+1/3; (lxxvii) y−x+2/3, y+1/3, z+1/3; (lxxviii) −y−1/3, −x−2/3, z+1/3; (lxxix) −y−1/3, −x+1/3, z+1/3; (lxxx) −y+2/3, −x+1/3, z+1/3; (lxxxi) x−1/3, x−y−2/3, z+1/3; (lxxxii) x−1/3, x−y+1/3, z+1/3; (lxxxiii) x+2/3, x−y+1/3, z+1/3; (lxxxiv) −x, −y, −z+1; (lxxxv) x, y−1, z; (lxxxvi) x+1, y, z; (lxxxvii) −y, x−y+1, z; (lxxxviii) −y+1, x−y+1, z; (lxxxix) y−x−1, −x−1, z; (xc) y−x−1, −x, z; (xci) y−x−1, y−1, z; (xcii) y−x−1, y, z; (xciii) −y, −x−1, z; (xciv) −y+1, −x, z; (xcv) x, x−y+1, z; (xcvi) x+1, x−y+1, z; (xcvii) y, y−x, −z+1; (xcviii) x−y, x, −z+1; (xcix) x−y, −y, −z+1; (100) y, x, −z+1; (101) −x, y−x, −z+1; (102) x−1, y, z; (103) x, y+1, z; (104) −x−1, −y, −z+1; (105) −x, −y+1, −z+1; (106) y−1, x, −z+1; (107) y, x+1, −z+1.

(S4P43_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8979 (5) Å	T = 298 K
c = 2.8289 (7) Å	Particle morphology: Pressure cell anvil material
V = 20.57 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.031	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 76.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 8.32 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 132.1 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 247.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.029	37 parameters
Rexp = 0.015	9 restraints
R(F^2) = 0.17705	(Δ/σ)max = 0.06
χ^2 = 4.000	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 3.51608 2: -1.00996 3: 1.62909 4: -0.377363 5: 0.687305 6: -0.296244 7: 0.392229 8: -0.165049 9: 0.194674 10: -0.106028 11: 8.209180E-0212: -9.164950E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.91437 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.208 (3)	P—PB2	4.204 (4)
PB1—PB2^i	4.208 (3)	P—PB2	4.088 (10)
PB1—PB2^ii	4.208 (3)	P—PB2	4.318 (9)
PB1—PB2^iii	4.208 (3)	P—PB2	4.088 (10)
PB1—PB2^iv	4.208 (3)	P—PB2	4.204 (4)
PB1—PB2^v	4.208 (3)	P—PB2	4.318 (9)
PB1—PB2	4.208 (3)	P—PB2	4.204 (4)
PB1—PB2	4.208 (3)	P—PB2	4.318 (9)
PB1—PB2	4.208 (3)	P—PB2	4.088 (10)
PB1—PB2	4.208 (3)	P—PB2	4.318 (9)
PB1—PB2	4.208 (3)	P—PB2	4.088 (10)
PB1—PB2	4.208 (3)	P—PB2	4.204 (4)
PB1—PB2	3.9971 (19)	P—P	3.847 (11)
PB1—PB2	3.874 (8)	P—P	4.223 (7)
PB1—PB2	4.116 (9)	P—P	4.223 (7)
PB1—PB2	4.116 (9)	P—P	4.223 (7)
PB1—PB2	3.9971 (19)	P—O1	1.519 (7)
PB1—PB2	3.874 (8)	P—O1^i	1.519 (7)
PB1—PB2	3.874 (8)	P—O1^ii	1.519 (7)
PB1—PB2	4.116 (9)	P—O1	3.465 (9)
PB1—PB2	3.9971 (19)	P—O1	3.280 (15)
PB1—PB2	3.874 (8)	P—O1	3.465 (9)
PB1—PB2	3.9971 (19)	P—O1	3.465 (9)
PB1—PB2	4.116 (9)	P—O1	3.465 (9)
PB1—PB2	4.116 (9)	P—O1	3.280 (15)
PB1—PB2	3.874 (8)	P—O1	3.280 (15)
PB1—PB2	3.9971 (19)	P—O1	3.465 (9)
PB1—PB2	3.9971 (19)	P—O1	3.465 (9)
PB1—PB2	4.116 (9)	P—O2^vi	4.243 (9)
PB1—PB2	3.874 (8)	P—O2	1.540 (4)
PB1—PB2	4.116 (9)	P—O2^vii	4.309 (9)
PB1—PB2	3.874 (8)	P—O2^i	1.540 (4)
PB1—PB2	3.9971 (19)	P—O2^viii	4.309 (9)
PB1—PB2	3.874 (8)	P—O2^ix	4.243 (9)
PB1—PB2	3.9971 (19)	P—O2^x	4.309 (9)
PB1—PB2	4.116 (9)	P—O2^xi	4.243 (9)
PB1—PB2	3.9971 (19)	P—O2^ii	1.540 (4)
PB1—PB2	4.116 (9)	P—O2^xii	4.243 (9)
PB1—PB2	3.874 (8)	P—O2^xiii	4.309 (9)
PB1—PB2	4.116 (9)	P—O2^iii	1.540 (4)
PB1—PB2	3.9971 (19)	P—O2^xiv	4.309 (9)
PB1—PB2	3.874 (8)	P—O2^iv	1.540 (4)
PB1—PB2	3.9971 (19)	P—O2^xv	4.243 (9)
PB1—PB2	3.874 (8)	P—O2^v	1.540 (4)
PB1—PB2	4.116 (9)	P—O2^xvi	4.243 (9)
PB1—PB2	3.874 (8)	P—O2^xvii	4.309 (9)
PB1—PB2	4.116 (9)	P—O2	3.631 (6)
PB1—PB2	3.9971 (19)	P—O2	3.631 (6)
PB1—P	3.442 (2)	P—O2	3.631 (6)
PB1—P	3.442 (2)	P—O2	3.631 (6)
PB1—P	3.442 (2)	P—O2	3.631 (6)
PB1—P	3.442 (2)	P—O2	3.631 (6)
PB1—P	3.442 (2)	P—O2	4.344 (10)
PB1—P	3.442 (2)	P—O2	4.278 (9)
PB1—O1	3.076 (8)	P—O2	4.278 (9)
PB1—O1	3.273 (16)	P—O2	4.344 (10)
PB1—O1	3.076 (8)	P—O2	4.278 (9)
PB1—O1	3.076 (8)	P—O2	4.344 (10)
PB1—O1	3.076 (8)	P—O2	4.344 (10)
PB1—O1	3.273 (16)	P—O2	4.278 (9)
PB1—O1	3.273 (16)	P—O2	4.278 (9)
PB1—O1	3.076 (8)	P—O2	4.344 (10)
PB1—O1	3.076 (8)	P—O2	4.344 (10)
PB1—O1	3.076 (8)	P—O2	4.278 (9)
PB1—O1	3.273 (16)	O1—PB1	3.076 (8)
PB1—O1	3.076 (8)	O1—PB1	3.273 (16)
PB1—O1	3.273 (16)	O1—PB1	3.076 (8)
PB1—O1	3.076 (8)	O1—PB2	2.387 (6)
PB1—O1	3.076 (8)	O1—PB2^i	2.378 (5)
PB1—O1	3.076 (8)	O1—PB2^ii	2.369 (5)
PB1—O1	3.076 (8)	O1—PB2^iii	2.378 (5)
PB1—O1	3.273 (16)	O1—PB2^iv	2.387 (6)
PB1—O2	2.566 (3)	O1—PB2^v	2.369 (5)
PB1—O2	2.566 (3)	O1—PB2	4.108 (7)
PB1—O2	2.566 (3)	O1—PB2	4.074 (15)
PB1—O2	2.566 (3)	O1—PB2	3.989 (10)
PB1—O2	2.566 (3)	O1—PB2	3.994 (10)
PB1—O2	2.566 (3)	O1—PB2	3.958 (13)
PB1—O2	2.566 (3)	O1—PB2	4.229 (12)
PB1—O2	2.566 (3)	O1—PB2	4.234 (13)
PB1—O2	2.566 (3)	O1—PB2	3.839 (15)
PB1—O2	2.566 (3)	O1—PB2	4.118 (8)
PB1—O2	2.566 (3)	O1—PB2	4.229 (12)
PB1—O2	2.566 (3)	O1—PB2	3.958 (13)
PB2—PB1	4.208 (3)	O1—PB2	3.994 (10)
PB2—PB1	4.116 (9)	O1—PB2	3.989 (10)
PB2—PB1	3.874 (8)	O1—PB2	4.074 (15)
PB2—PB1	3.9971 (19)	O1—PB2	4.108 (7)
PB2—PB2^i	0.31 (2)	O1—PB2	4.118 (8)
PB2—PB2^ii	0.31 (2)	O1—PB2	3.839 (15)
PB2—PB2^iii	0.178 (12)	O1—PB2	4.234 (13)
PB2—PB2^iv	0.178 (12)	O1—P	1.519 (7)
PB2—PB2^v	0.36 (3)	O1—P	3.465 (9)
PB2—PB2	3.86 (2)	O1—P	3.280 (15)
PB2—PB2	3.326 (18)	O1—P	3.465 (9)
PB2—PB2	3.605 (4)	O1—O1^i	0.23 (3)
PB2—PB2	3.591 (3)	O1—O1^ii	0.23 (3)
PB2—PB2	3.454 (9)	O1—O1	3.286 (18)
PB2—PB2	3.724 (10)	O1—O1	2.88 (3)
PB2—PB2	3.724 (10)	O1—O1	3.286 (18)
PB2—PB2	3.591 (3)	O1—O1	3.278 (16)
PB2—PB2	3.454 (9)	O1—O1	3.081 (8)
PB2—PB2	3.859 (19)	O1—O1	3.081 (8)
PB2—PB2	3.463 (8)	O1—O1	3.081 (8)
PB2—PB2	3.463 (8)	O1—O1	3.081 (8)
PB2—PB2	3.732 (11)	O1—O1	3.278 (16)
PB2—PB2	3.321 (18)	O1—O2	2.575 (11)
PB2—PB2	3.732 (11)	O1—O2^i	2.463 (6)
PB2—PB2	3.587 (3)	O1—O2^ii	2.458 (7)
PB2—PB2	3.587 (3)	O1—O2^iii	2.463 (6)
PB2—PB2	3.587 (3)	O1—O2^iv	2.575 (11)
PB2—P	3.885 (7)	O1—O2^v	2.458 (7)
PB2—P	4.204 (4)	O1—O2	3.330 (12)
PB2—P	4.318 (9)	O1—O2	3.244 (11)
PB2—P	4.088 (10)	O1—O2	3.330 (15)
PB2—P	3.3164 (17)	O1—O2	3.226 (14)
PB2—P	3.459 (10)	O1—O2	3.140 (18)
PB2—P	3.167 (11)	O1—O2	3.417 (18)
PB2—O1	2.387 (6)	O1—O2	3.226 (14)
PB2—O1^i	2.369 (5)	O1—O2	3.330 (15)
PB2—O1^ii	2.378 (5)	O1—O2	3.244 (11)
PB2—O1	4.108 (7)	O1—O2	3.330 (12)
PB2—O1	4.074 (15)	O1—O2	3.417 (18)
PB2—O1	3.989 (10)	O1—O2	3.140 (18)
PB2—O1	4.118 (8)	O2—PB1	2.566 (3)
PB2—O1	4.234 (13)	O2—PB2	2.910 (15)
PB2—O1	3.839 (15)	O2—PB2	2.633 (15)
PB2—O1	3.958 (13)	O2—PB2	2.650 (18)
PB2—O1	4.229 (12)	O2—PB2	2.897 (17)
PB2—O1	3.994 (10)	O2—PB2	2.922 (15)
PB2—O2	2.927 (7)	O2—PB2	2.647 (14)
PB2—O2	2.744 (8)	O2—PB2	2.999 (18)
PB2—O2	2.842 (4)	O2—PB2	2.549 (18)
PB2—O2	2.835 (4)	O2—PB2	2.735 (14)
PB2—O2	2.930 (7)	O2—PB2	2.807 (14)
PB2—O2	2.747 (8)	O2—PB2	2.748 (14)
PB2—O2	2.910 (15)	O2—PB2	2.821 (14)
PB2—O2	2.633 (15)	O2—PB2	2.927 (7)
PB2—O2	2.647 (14)	O2—PB2	2.842 (4)
PB2—O2	2.922 (15)	O2—PB2	2.744 (8)
PB2—O2	2.897 (17)	O2—PB2	2.835 (4)
PB2—O2	2.650 (18)	O2—PB2	2.930 (7)
PB2—O2	2.999 (18)	O2—PB2	2.747 (8)
PB2—O2	2.549 (18)	O2—P^xviii	4.309 (9)
PB2—O2	2.807 (14)	O2—P	1.540 (4)
PB2—O2	2.735 (14)	O2—P^xix	4.243 (9)
PB2—O2	2.748 (14)	O2—P	3.631 (6)
PB2—O2	2.821 (14)	O2—P	4.344 (10)
P—PB1	3.442 (2)	O2—P	4.278 (9)
P—PB1	3.442 (2)	O2—O1	2.575 (11)
P—PB1	3.442 (2)	O2—O1^i	2.458 (7)
P—PB2	3.885 (7)	O2—O1^ii	2.463 (6)
P—PB2^i	3.885 (7)	O2—O1	3.330 (12)
P—PB2^ii	3.885 (7)	O2—O1	3.244 (11)
P—PB2^iii	3.885 (7)	O2—O1	3.417 (18)
P—PB2^iv	3.885 (7)	O2—O1	3.140 (18)
P—PB2^v	3.885 (7)	O2—O1	3.226 (14)
P—PB2	3.3164 (17)	O2—O1	3.330 (15)
P—PB2	3.459 (10)	O2—O2^i	2.512 (6)
P—PB2	3.167 (11)	O2—O2^viii	2.928 (6)
P—PB2	3.167 (11)	O2—O2^xi	2.928 (6)
P—PB2	3.3164 (17)	O2—O2^ii	2.512 (6)
P—PB2	3.459 (10)	O2—O2^xiii	2.979 (15)
P—PB2	3.459 (10)	O2—O2^iii	2.458 (15)
P—PB2	3.167 (11)	O2—O2^iv	0.10 (3)
P—PB2	3.3164 (17)	O2—O2^v	2.562 (14)
P—PB2	3.459 (10)	O2—O2^xvi	2.875 (14)
P—PB2	3.3164 (17)	O2—O2	4.375 (18)
P—PB2	3.167 (11)	O2—O2	4.039 (6)
P—PB2	3.167 (11)	O2—O2	4.244 (17)
P—PB2	3.459 (10)	O2—O2	3.163 (5)
P—PB2	3.3164 (17)	O2—O2	3.163 (5)
P—PB2	3.3164 (17)	O2—O2	3.204 (12)
P—PB2	3.167 (11)	O2—O2	4.309 (4)
P—PB2	3.459 (10)	O2—O2	4.037 (6)
P—PB2	4.088 (10)	O2—O2	4.309 (4)
P—PB2	4.318 (9)	O2—O2	3.122 (11)
P—PB2	4.204 (4)	O2—O2	4.216 (5)
P—PB2	4.318 (9)	O2—O2	4.216 (5)
P—PB2	4.204 (4)	O2—O2	4.180 (10)
P—PB2	4.088 (10)	O2—O2	4.252 (11)
PB2^i—PB2—PB2^ii	60.0	O1^ii—P—O2	107.3 (4)
PB2^i—PB2—PB2^iii	90.0	O1^ii—P—O2^i	106.9 (4)
PB2^i—PB2—PB2^iv	30.0000 (9)	O1^ii—P—O2^ii	114.7 (6)
PB2^i—PB2—PB2^v	30.0	O1^ii—P—O2^iii	114.7 (6)
PB2^ii—PB2—PB2^iii	30.0000 (9)	O1^ii—P—O2^iv	106.9 (4)
PB2^ii—PB2—PB2^iv	90.0	O1^ii—P—O2^v	107.3 (4)
PB2^ii—PB2—PB2^v	30.0	O2—P—O2^i	109.3 (2)
PB2^iii—PB2—PB2^iv	120.0000 (13)	O2—P—O2^ii	109.3 (2)
PB2^iii—PB2—PB2^v	60.0000 (5)	O2—P—O2^iii	105.9 (9)
PB2^iv—PB2—PB2^v	60.0000 (5)	O2—P—O2^iv	3.9 (10)
O1—P—O1^i	8.7 (11)	O2—P—O2^v	112.6 (9)
O1—P—O1^ii	8.7 (11)	O2^i—P—O2^ii	109.3 (2)
O1—P—O2	114.7 (6)	O2^i—P—O2^iii	112.6 (9)
O1—P—O2^i	107.3 (4)	O2^i—P—O2^iv	105.9 (9)
O1—P—O2^ii	106.9 (4)	O2^i—P—O2^v	3.9 (10)
O1—P—O2^iii	107.3 (4)	O2^ii—P—O2^iii	3.9 (10)
O1—P—O2^iv	114.7 (6)	O2^ii—P—O2^iv	112.6 (9)
O1—P—O2^v	106.9 (4)	O2^ii—P—O2^v	105.9 (9)
O1^i—P—O1^ii	8.7 (11)	O2^iii—P—O2^iv	109.3 (2)
O1^i—P—O2	106.9 (4)	O2^iii—P—O2^v	109.3 (2)
O1^i—P—O2^i	114.7 (6)	O2^iv—P—O2^v	109.3 (2)
O1^i—P—O2^ii	107.3 (4)	P—O1—O1^i	85.7 (5)
O1^i—P—O2^iii	106.9 (4)	P—O1—O1^ii	85.7 (5)
O1^i—P—O2^iv	107.3 (4)	O1^i—O1—O1^ii	60.0
O1^i—P—O2^v	114.7 (6)	P—O2—O2^iv	88.1 (5)

Symmetry codes: (i) y−x, −x, −z; (ii) −y, x−y, z; (iii) x, y, −z; (iv) y−x, −x, z; (v) −y, x−y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) y−x, −x+1, −z; (ix) y−x+1, −x+1, −z; (x) −y−1, x−y−1, z; (xi) −y−1, x−y, z; (xii) x−1, y−1, −z; (xiii) x−1, y, −z; (xiv) y−x, −x−1, z; (xv) y−x+1, −x, z; (xvi) −y, x−y+1, −z; (xvii) −y+1, x−y+1, −z; (xviii) x−1, y, z; (xix) x, y+1, z.

(S4P43_phase_3)

Crystal data

Ni	anvil material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5409 (5) Å	Particle morphology: Component of pressure cell, not sample
V = 44.40 (1) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.031	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 76.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 8.32 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 132.1 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 247.7 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.029	37 parameters
Rexp = 0.015	9 restraints
R(F^2) = 0.17705	(Δ/σ)max = 0.06
χ^2 = 4.000	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 3.51608 2: -1.00996 3: 1.62909 4: -0.377363 5: 0.687305 6: -0.296244 7: 0.392229 8: -0.165049 9: 0.194674 10: -0.106028 11: 8.209180E-0212: -9.164950E-03
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.91437 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

(S4P55TISO_phase_1)

Crystal data

O8P2Pb3	Z = 3
Mr = 811.54	none
Trigonal, R3m	? radiation
Hall symbol: -R32''-P3*2	T = 298 K
a = 5.4041 (3) Å	Particle morphology: plate
c = 19.9364 (15) Å	irregular, 6 × 6 mm
V = 504.22 (5) Å^3

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.058	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 76.2 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 11.19 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 151.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 332.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.044	34 parameters
Rexp = 0.033	4 restraints
R(F^2) = 0.13667	(Δ/σ)max = 0.01
χ^2 = 1.796	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.36252 2: -0.369554 3: 0.748163 4: -0.172031 5: 0.364863 6: -0.139767 7: 0.200747 8: -6.467880E-02 9: 9.089620E-0210: -3.771570E-0211: 3.153040E-0212: -1.410160E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.88919 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
PB1	0.0	0.0	0.0	0.0195 (13)*
PB2	0.0	0.0	0.2097 (2)	0.0195 (13)*
P	0.0	0.0	0.4043 (4)	0.0107 (17)*
O1	0.0	0.0	0.3281 (3)	0.0174 (12)*
O2	−0.1544 (5)	0.1544 (5)	0.43034 (18)	0.0174 (12)*

Geometric parameters (Å, º)

PB1—PB2	4.180 (4)	P—O1^xv	3.384 (4)
PB1—PB2^i	4.180 (4)	P—O1^xvi	3.384 (4)
PB1—PB2^ii	3.977 (3)	P—O1^xvii	3.384 (4)
PB1—PB2^iii	3.977 (3)	P—O2^xxiii	4.246 (4)
PB1—PB2^iv	3.977 (3)	P—O2	1.536 (5)
PB1—PB2^v	3.977 (3)	P—O2^xxiv	4.246 (4)
PB1—PB2^vi	3.977 (3)	P—O2^xxv	1.536 (5)
PB1—PB2^vii	3.977 (3)	P—O2^xxvi	4.246 (4)
PB1—P^ii	3.426 (4)	P—O2^xxvii	4.246 (4)
PB1—P^iii	3.426 (4)	P—O2^xxviii	4.246 (4)
PB1—P^iv	3.426 (4)	P—O2^xxix	4.246 (4)
PB1—P^v	3.426 (4)	P—O2^xxx	1.536 (5)
PB1—P^vi	3.426 (4)	P—O2^xxii	3.600 (9)
PB1—P^vii	3.426 (4)	P—O2^xxxi	3.600 (9)
PB1—O1^ii	3.1218 (3)	P—O2^xxxii	3.600 (9)
PB1—O1^iii	3.1218 (3)	P—O2^xv	4.304 (7)
PB1—O1^iv	3.1218 (3)	P—O2^xvii	4.304 (7)
PB1—O1^v	3.1218 (3)	P—O2^xviii	4.304 (7)
PB1—O1^vi	3.1218 (3)	P—O2^xix	4.304 (7)
PB1—O1^vii	3.1218 (3)	P—O2^xx	4.304 (7)
PB1—O2^iii	2.558 (4)	P—O2^xxi	4.304 (7)
PB1—O2^viii	2.558 (4)	O1—PB1^xii	3.1218 (3)
PB1—O2^ix	2.558 (4)	O1—PB1^xiii	3.1218 (3)
PB1—O2^vi	2.558 (4)	O1—PB1^xiv	3.1218 (3)
PB1—O2^x	2.558 (4)	O1—PB2	2.362 (7)
PB1—O2^xi	2.558 (4)	O1—PB2^xv	4.042 (5)
PB2—PB1	4.180 (4)	O1—PB2^xvi	4.042 (5)
PB2—PB1^xii	3.977 (3)	O1—PB2^xvii	4.042 (5)
PB2—PB1^xiii	3.977 (3)	O1—P	1.519 (11)
PB2—PB1^xiv	3.977 (3)	O1—P^xv	3.384 (4)
PB2—PB2^v	3.560 (4)	O1—P^xvi	3.384 (4)
PB2—PB2^vi	3.560 (4)	O1—P^xvii	3.384 (4)
PB2—PB2^vii	3.560 (4)	O1—O1^xv	3.1270 (8)
PB2—P	3.880 (11)	O1—O1^xvi	3.1270 (8)
PB2—P^ii	4.169 (7)	O1—O1^xvii	3.1270 (8)
PB2—P^iii	4.169 (7)	O1—O2	2.499 (7)
PB2—P^iv	4.169 (7)	O1—O2^xxv	2.499 (7)
PB2—P^xv	3.292 (3)	O1—O2^xxx	2.499 (7)
PB2—P^xvi	3.292 (3)	O1—O2^xv	3.265 (4)
PB2—P^xvii	3.292 (3)	O1—O2^xvii	3.265 (4)
PB2—O1	2.362 (7)	O1—O2^xviii	3.265 (4)
PB2—O1^xv	4.042 (5)	O1—O2^xix	3.265 (4)
PB2—O1^xvi	4.042 (5)	O1—O2^xx	3.265 (4)
PB2—O1^xvii	4.042 (5)	O1—O2^xxi	3.265 (4)
PB2—O2^iii	2.801 (5)	O2—PB1^xiii	2.558 (4)
PB2—O2^viii	2.801 (5)	O2—PB2^xv	2.7562 (11)
PB2—O2^ix	2.801 (5)	O2—PB2^xvii	2.7562 (11)
PB2—O2^xv	2.7562 (11)	O2—PB2^xiii	2.801 (5)
PB2—O2^xvii	2.7562 (11)	O2—P^xxxiii	4.246 (4)
PB2—O2^xviii	2.7562 (11)	O2—P	1.536 (5)
PB2—O2^xix	2.7562 (11)	O2—P^xxxiv	4.246 (4)
PB2—O2^xx	2.7562 (11)	O2—P^xxii	3.600 (9)
PB2—O2^xxi	2.7562 (11)	O2—P^xv	4.304 (7)
P—PB1^xii	3.426 (4)	O2—P^xvii	4.304 (7)
P—PB1^xiii	3.426 (4)	O2—O1	2.499 (7)
P—PB1^xiv	3.426 (4)	O2—O1^xv	3.265 (4)
P—PB2	3.880 (11)	O2—O1^xvii	3.265 (4)
P—PB2^xv	3.292 (3)	O2—O2^xxv	2.504 (8)
P—PB2^xvi	3.292 (3)	O2—O2^xxvi	2.900 (8)
P—PB2^xvii	3.292 (3)	O2—O2^xxix	2.900 (8)
P—PB2^xii	4.169 (7)	O2—O2^xxx	2.504 (8)
P—PB2^xiii	4.169 (7)	O2—O2^xxxv	4.268 (6)
P—PB2^xiv	4.169 (7)	O2—O2^xxii	4.009 (9)
P—P^xxii	3.816 (17)	O2—O2^xxxvi	4.268 (6)
P—P^xv	4.212 (11)	O2—O2^xxxi	3.131 (7)
P—P^xvi	4.212 (11)	O2—O2^xxxii	3.131 (7)
P—P^xvii	4.212 (11)	O2—O2^xviii	4.215 (7)
P—O1	1.519 (11)	O2—O2^xxi	4.215 (7)
O1—P—O2	109.8 (3)	O2—P—O2^xxv	109.2 (3)
O1—P—O2^xxv	109.8 (3)	O2—P—O2^xxx	109.2 (3)
O1—P—O2^xxx	109.8 (3)	O2^xxv—P—O2^xxx	109.2 (3)

Symmetry codes: (i) −x, −y, −z; (ii) x−2/3, y−1/3, z−1/3; (iii) x+1/3, y−1/3, z−1/3; (iv) x+1/3, y+2/3, z−1/3; (v) −x−2/3, −y−1/3, −z+2/3; (vi) −x−2/3, −y+2/3, −z+2/3; (vii) −x+1/3, −y+2/3, −z+2/3; (viii) −y+1/3, x−y+2/3, z−1/3; (ix) y−x−2/3, −x−1/3, z−1/3; (x) y−2/3, y−x−1/3, −z+2/3; (xi) x−y+1/3, x+2/3, −z+2/3; (xii) x−1/3, y−2/3, z+1/3; (xiii) x−1/3, y+1/3, z+1/3; (xiv) x+2/3, y+1/3, z+1/3; (xv) −x−1/3, −y−2/3, −z+1/3; (xvi) −x+2/3, −y−2/3, −z+1/3; (xvii) −x+2/3, −y+1/3, −z+1/3; (xviii) y−1/3, y−x−2/3, −z+1/3; (xix) y+2/3, y−x−2/3, −z+1/3; (xx) x−y+2/3, x−2/3, −z+1/3; (xxi) x−y+2/3, x+1/3, −z+1/3; (xxii) −x, −y, −z+1; (xxiii) x, y−1, z; (xxiv) x+1, y, z; (xxv) −y, x−y, z; (xxvi) −y, x−y+1, z; (xxvii) −y+1, x−y+1, z; (xxviii) y−x−1, −x−1, z; (xxix) y−x−1, −x, z; (xxx) y−x, −x, z; (xxxi) y, y−x, −z+1; (xxxii) x−y, x, −z+1; (xxxiii) x−1, y, z; (xxxiv) x, y+1, z; (xxxv) −x−1, −y, −z+1; (xxxvi) −x, −y+1, −z+1.

(S4P55TISO_phase_2)

Crystal data

CW	Z = 1
Mr = 195.86	anvil material not at centre of diffractometer: cell parameters meaningless
Hexagonal, P6m2	? radiation
a = 2.8945 (7) Å	T = 298 K
c = 2.8293 (11) Å	Particle morphology: Pressure cell anvil material
V = 20.53 (1) Å^3	irregular, 6 × 6 mm

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.058	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 76.2 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 11.19 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 151.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 332.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.044	34 parameters
Rexp = 0.033	4 restraints
R(F^2) = 0.13667	(Δ/σ)max = 0.01
χ^2 = 1.796	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.36252 2: -0.369554 3: 0.748163 4: -0.172031 5: 0.364863 6: -0.139767 7: 0.200747 8: -6.467880E-02 9: 9.089620E-0210: -3.771570E-0211: 3.153040E-0212: -1.410160E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.88919 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W	0.0	0.0	0.0	0.025*
C	0.66667	0.33333	0.5	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.180 (4)	P—O1	3.384 (4)
PB1—PB2	4.180 (4)	P—O1	3.384 (4)
PB1—PB2	3.977 (3)	P—O1	3.384 (4)
PB1—PB2	3.977 (3)	P—O2^i	4.246 (4)
PB1—PB2	3.977 (3)	P—O2	1.536 (5)
PB1—PB2	3.977 (3)	P—O2^ii	4.246 (4)
PB1—PB2	3.977 (3)	P—O2^iii	1.536 (5)
PB1—PB2	3.977 (3)	P—O2^iv	4.246 (4)
PB1—P	3.426 (4)	P—O2^v	4.246 (4)
PB1—P	3.426 (4)	P—O2^vi	4.246 (4)
PB1—P	3.426 (4)	P—O2^vii	4.246 (4)
PB1—P	3.426 (4)	P—O2^viii	1.536 (5)
PB1—P	3.426 (4)	P—O2	3.600 (9)
PB1—P	3.426 (4)	P—O2	3.600 (9)
PB1—O1	3.1218 (3)	P—O2	3.600 (9)
PB1—O1	3.1218 (3)	P—O2	4.304 (7)
PB1—O1	3.1218 (3)	P—O2	4.304 (7)
PB1—O1	3.1218 (3)	P—O2	4.304 (7)
PB1—O1	3.1218 (3)	P—O2	4.304 (7)
PB1—O1	3.1218 (3)	P—O2	4.304 (7)
PB1—O2	2.558 (4)	P—O2	4.304 (7)
PB1—O2	2.558 (4)	O1—PB1	3.1218 (3)
PB1—O2	2.558 (4)	O1—PB1	3.1218 (3)
PB1—O2	2.558 (4)	O1—PB1	3.1218 (3)
PB1—O2	2.558 (4)	O1—PB2	2.362 (7)
PB1—O2	2.558 (4)	O1—PB2	4.042 (5)
PB2—PB1	4.180 (4)	O1—PB2	4.042 (5)
PB2—PB1	3.977 (3)	O1—PB2	4.042 (5)
PB2—PB1	3.977 (3)	O1—P	1.519 (11)
PB2—PB1	3.977 (3)	O1—P	3.384 (4)
PB2—PB2	3.560 (4)	O1—P	3.384 (4)
PB2—PB2	3.560 (4)	O1—P	3.384 (4)
PB2—PB2	3.560 (4)	O1—O1	3.1270 (8)
PB2—P	3.880 (11)	O1—O1	3.1270 (8)
PB2—P	4.169 (7)	O1—O1	3.1270 (8)
PB2—P	4.169 (7)	O1—O2	2.499 (7)
PB2—P	4.169 (7)	O1—O2^iii	2.499 (7)
PB2—P	3.292 (3)	O1—O2^viii	2.499 (7)
PB2—P	3.292 (3)	O1—O2	3.265 (4)
PB2—P	3.292 (3)	O1—O2	3.265 (4)
PB2—O1	2.362 (7)	O1—O2	3.265 (4)
PB2—O1	4.042 (5)	O1—O2	3.265 (4)
PB2—O1	4.042 (5)	O1—O2	3.265 (4)
PB2—O1	4.042 (5)	O1—O2	3.265 (4)
PB2—O2	2.801 (5)	O2—PB1	2.558 (4)
PB2—O2	2.801 (5)	O2—PB2	2.7562 (11)
PB2—O2	2.801 (5)	O2—PB2	2.7562 (11)
PB2—O2	2.7562 (11)	O2—PB2	2.801 (5)
PB2—O2	2.7562 (11)	O2—P^ix	4.246 (4)
PB2—O2	2.7562 (11)	O2—P	1.536 (5)
PB2—O2	2.7562 (11)	O2—P^x	4.246 (4)
PB2—O2	2.7562 (11)	O2—P	3.600 (9)
PB2—O2	2.7562 (11)	O2—P	4.304 (7)
P—PB1	3.426 (4)	O2—P	4.304 (7)
P—PB1	3.426 (4)	O2—O1	2.499 (7)
P—PB1	3.426 (4)	O2—O1	3.265 (4)
P—PB2	3.880 (11)	O2—O1	3.265 (4)
P—PB2	3.292 (3)	O2—O2^iii	2.504 (8)
P—PB2	3.292 (3)	O2—O2^iv	2.900 (8)
P—PB2	3.292 (3)	O2—O2^vii	2.900 (8)
P—PB2	4.169 (7)	O2—O2^viii	2.504 (8)
P—PB2	4.169 (7)	O2—O2	4.268 (6)
P—PB2	4.169 (7)	O2—O2	4.009 (9)
P—P	3.816 (17)	O2—O2	4.268 (6)
P—P	4.212 (11)	O2—O2	3.131 (7)
P—P	4.212 (11)	O2—O2	3.131 (7)
P—P	4.212 (11)	O2—O2	4.215 (7)
P—O1	1.519 (11)	O2—O2	4.215 (7)
O1—P—O2	109.8 (3)	O2—P—O2^iii	109.2 (3)
O1—P—O2^iii	109.8 (3)	O2—P—O2^viii	109.2 (3)
O1—P—O2^viii	109.8 (3)	O2^iii—P—O2^viii	109.2 (3)

Symmetry codes: (i) x, y−1, z; (ii) x+1, y, z; (iii) y−x, −x, −z; (iv) y−x, −x+1, −z; (v) y−x+1, −x+1, −z; (vi) −y−1, x−y−1, z; (vii) −y−1, x−y, z; (viii) −y, x−y, z; (ix) x−1, y, z; (x) x, y+1, z.

(S4P55TISO_phase_3)

Crystal data

Ni	anvil material not at centre of diffractometer: cell parameters meaningless
Mr = 58.71	? radiation
Cubic, Fm3m	T = 298 K
a = 3.5355 (8) Å	Particle morphology: Component of pressure cell, not sample
V = 44.19 (4) Å^3	irregular, 6 × 6 mm
Z = 4

Data collection

None diffractometer	2θfixed = 90.00
Radiation source: spallation source, PEARL beamline ISIS Neutron Facility	Distance from source to specimen: 13200 mm
Specimen mounting: Paris-Edinburgh pressure cell, using standard WC anvils.	Distance from specimen to detector: 600 mm
Scan method: time of flight

Refinement

Least-squares matrix: full	Excluded region(s): d < 0.585 Angstrom (no useful data), d > 3.63 Angstrom (no useful data)
Rp = 0.058	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 76.2 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 11.19 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 151.8 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2363 #2 (bet-0) = 0.023120 #3 (bet-1) = 0.030770 #4 (sig-0) = 0.0 #5 (sig-1) = 332.6 #6 (sig-2) = 1.8 #7 (gam-0) = 0.00 #8 (gam-1) = 3.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.044	34 parameters
Rexp = 0.033	4 restraints
R(F^2) = 0.13667	(Δ/σ)max = 0.01
χ^2 = 1.796	Background function: GSAS Background function number 2 with 12 terms. Cosine Fourier series 1: 1.36252 2: -0.369554 3: 0.748163 4: -0.172031 5: 0.364863 6: -0.139767 7: 0.200747 8: -6.467880E-02 9: 9.089620E-0210: -3.771570E-0211: 3.153040E-0212: -1.410160E-04
2524 data points	Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.88919 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000, March-Dollase AXIS 1 Ratio= 1.00000 h= 0.000 k= 0.000 l= 1.000

Special details

Experimental. High-pressure neutron powder diffraction using the time-of-flight technique. Pressure cell in use: Paris-Edinburgh opposed anvil device, with _{90 mm^{3 sample volume.}}

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º)

PB1—PB2	4.180 (4)	P—O1^xv	3.384 (4)
PB1—PB2^i	4.180 (4)	P—O1^xvi	3.384 (4)
PB1—PB2^ii	3.977 (3)	P—O1^xvii	3.384 (4)
PB1—PB2^iii	3.977 (3)	P—O2^xxiii	4.246 (4)
PB1—PB2^iv	3.977 (3)	P—O2	1.536 (5)
PB1—PB2^v	3.977 (3)	P—O2^xxiv	4.246 (4)
PB1—PB2^vi	3.977 (3)	P—O2^xxv	1.536 (5)
PB1—PB2^vii	3.977 (3)	P—O2^xxvi	4.246 (4)
PB1—P^ii	3.426 (4)	P—O2^xxvii	4.246 (4)
PB1—P^iii	3.426 (4)	P—O2^xxviii	4.246 (4)
PB1—P^iv	3.426 (4)	P—O2^xxix	4.246 (4)
PB1—P^v	3.426 (4)	P—O2^xxx	1.536 (5)
PB1—P^vi	3.426 (4)	P—O2^xxii	3.600 (9)
PB1—P^vii	3.426 (4)	P—O2^xxxi	3.600 (9)
PB1—O1^ii	3.1218 (3)	P—O2^xxxii	3.600 (9)
PB1—O1^iii	3.1218 (3)	P—O2^xv	4.304 (7)
PB1—O1^iv	3.1218 (3)	P—O2^xvii	4.304 (7)
PB1—O1^v	3.1218 (3)	P—O2^xviii	4.304 (7)
PB1—O1^vi	3.1218 (3)	P—O2^xix	4.304 (7)
PB1—O1^vii	3.1218 (3)	P—O2^xx	4.304 (7)
PB1—O2^iii	2.558 (4)	P—O2^xxi	4.304 (7)
PB1—O2^viii	2.558 (4)	O1—PB1^xii	3.1218 (3)
PB1—O2^ix	2.558 (4)	O1—PB1^xiii	3.1218 (3)
PB1—O2^vi	2.558 (4)	O1—PB1^xiv	3.1218 (3)
PB1—O2^x	2.558 (4)	O1—PB2	2.362 (7)
PB1—O2^xi	2.558 (4)	O1—PB2^xv	4.042 (5)
PB2—PB1	4.180 (4)	O1—PB2^xvi	4.042 (5)
PB2—PB1^xii	3.977 (3)	O1—PB2^xvii	4.042 (5)
PB2—PB1^xiii	3.977 (3)	O1—P	1.519 (11)
PB2—PB1^xiv	3.977 (3)	O1—P^xv	3.384 (4)
PB2—PB2^v	3.560 (4)	O1—P^xvi	3.384 (4)
PB2—PB2^vi	3.560 (4)	O1—P^xvii	3.384 (4)
PB2—PB2^vii	3.560 (4)	O1—O1^xv	3.1270 (8)
PB2—P	3.880 (11)	O1—O1^xvi	3.1270 (8)
PB2—P^ii	4.169 (7)	O1—O1^xvii	3.1270 (8)
PB2—P^iii	4.169 (7)	O1—O2	2.499 (7)
PB2—P^iv	4.169 (7)	O1—O2^xxv	2.499 (7)
PB2—P^xv	3.292 (3)	O1—O2^xxx	2.499 (7)
PB2—P^xvi	3.292 (3)	O1—O2^xv	3.265 (4)
PB2—P^xvii	3.292 (3)	O1—O2^xvii	3.265 (4)
PB2—O1	2.362 (7)	O1—O2^xviii	3.265 (4)
PB2—O1^xv	4.042 (5)	O1—O2^xix	3.265 (4)
PB2—O1^xvi	4.042 (5)	O1—O2^xx	3.265 (4)
PB2—O1^xvii	4.042 (5)	O1—O2^xxi	3.265 (4)
PB2—O2^iii	2.801 (5)	O2—PB1^xiii	2.558 (4)
PB2—O2^viii	2.801 (5)	O2—PB2^xv	2.7562 (11)
PB2—O2^ix	2.801 (5)	O2—PB2^xvii	2.7562 (11)
PB2—O2^xv	2.7562 (11)	O2—PB2^xiii	2.801 (5)
PB2—O2^xvii	2.7562 (11)	O2—P^xxxiii	4.246 (4)
PB2—O2^xviii	2.7562 (11)	O2—P	1.536 (5)
PB2—O2^xix	2.7562 (11)	O2—P^xxxiv	4.246 (4)
PB2—O2^xx	2.7562 (11)	O2—P^xxii	3.600 (9)
PB2—O2^xxi	2.7562 (11)	O2—P^xv	4.304 (7)
P—PB1^xii	3.426 (4)	O2—P^xvii	4.304 (7)
P—PB1^xiii	3.426 (4)	O2—O1	2.499 (7)
P—PB1^xiv	3.426 (4)	O2—O1^xv	3.265 (4)
P—PB2	3.880 (11)	O2—O1^xvii	3.265 (4)
P—PB2^xv	3.292 (3)	O2—O2^xxv	2.504 (8)
P—PB2^xvi	3.292 (3)	O2—O2^xxvi	2.900 (8)
P—PB2^xvii	3.292 (3)	O2—O2^xxix	2.900 (8)
P—PB2^xii	4.169 (7)	O2—O2^xxx	2.504 (8)
P—PB2^xiii	4.169 (7)	O2—O2^xxxv	4.268 (6)
P—PB2^xiv	4.169 (7)	O2—O2^xxii	4.009 (9)
P—P^xxii	3.816 (17)	O2—O2^xxxvi	4.268 (6)
P—P^xv	4.212 (11)	O2—O2^xxxi	3.131 (7)
P—P^xvi	4.212 (11)	O2—O2^xxxii	3.131 (7)
P—P^xvii	4.212 (11)	O2—O2^xviii	4.215 (7)
P—O1	1.519 (11)	O2—O2^xxi	4.215 (7)
O1—P—O2	109.8 (3)	O2—P—O2^xxv	109.2 (3)
O1—P—O2^xxv	109.8 (3)	O2—P—O2^xxx	109.2 (3)
O1—P—O2^xxx	109.8 (3)	O2^xxv—P—O2^xxx	109.2 (3)

Symmetry codes: (i) −x, −y, −z; (ii) x−1, y−1/2, z−1/2; (iii) x, y−1/2, z−1/2; (iv) x, y+1/2, z−1/2; (v) −x−1/2, −y−1, −z+1/2; (vi) −x−1/2, −y, −z+1/2; (vii) −x+1/2, −y, −z+1/2; (viii) z, x+1/2, y−1/2; (ix) y−1, z−1/2, x−1/2; (x) −z−1/2, −x−1, −y+1/2; (xi) −y+1/2, −z, −x+1/2; (xii) x−1/2, y−1, z+1/2; (xiii) x−1/2, y, z+1/2; (xiv) x+1/2, y, z+1/2; (xv) −x−1, −y−1/2, −z+1/2; (xvi) −x, −y−1/2, −z+1/2; (xvii) −x, −y+1/2, −z+1/2; (xviii) −z−1, −x−1/2, −y+1/2; (xix) −z, −x−1/2, −y+1/2; (xx) −y, −z−1/2, −x+1/2; (xxi) −y, −z+1/2, −x+1/2; (xxii) −x, −y, −z+1; (xxiii) x, y−1, z; (xxiv) x+1, y, z; (xxv) z, x, y; (xxvi) z, x+1, y; (xxvii) z+1, x+1, y; (xxviii) y−1, z−1, x; (xxix) y−1, z, x; (xxx) y, z, x; (xxxi) −z, −x, −y+1; (xxxii) −y, −z, −x+1; (xxxiii) x−1, y, z; (xxxiv) x, y+1, z; (xxxv) −x−1, −y, −z+1; (xxxvi) −x, −y+1, −z+1.