A new high-pressure polymorph of phosphoric acid

The high-pressure structural behaviour of phosphoric acid is described. A compression study of the monoclinic phase, using neutron powder diffraction and X-ray single-crystal diffraction, shows that it converts to a previously unobserved orthorhombic phase on decompression. Compression of this new phase is reported up to 6.3 GPa. The orthorhombic phase is found to be more efficiently packed, with reduced void space, resulting in a larger bulk modulus. Molecule–molecule interaction energies reveal a more extensive network of increased attractive forces in the orthorhombic form relative to the monoclinic form, suggesting greater thermodynamic stability.

Computing details

Data collection: Custom ISIS software for Phosphoric_acid_I_0.01_GPa. Cell refinement: GSAS for Phosphoric_acid_I_0.01_GPa. Program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) for Phosphoric_acid_I_0.5_GPa_S_xtal, Phosphoric_acid_II_1.8_GPa_S_Xtal.

Phosphoric acid (Phosphoric_acid_I_0.5_GPa_S_xtal)

Crystal data

H3O4P	F(000) = 200
Mr = 97.99	Dx = 2.076 Mg m^−3
Monoclinic, P21/c	Melting point: 315.5 K K
Hall symbol: -P 2ybc	Mo Kα radiation, λ = 0.71073 Å
a = 5.707 (2) Å	Cell parameters from 24 reflections
b = 4.820 (2) Å	θ = 3.6–15.3°
c = 11.436 (2) Å	µ = 0.69 mm^−1
β = 94.75 (5)°	T = 293 K
V = 313.49 (18) Å^3	Block, colourless
Z = 4	0.2 × 0.18 × 0.08 mm

Data collection

Nonius CAD4 diffractometer	294 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.086
Graphite monochromator	θmax = 39.1°, θmin = 3.6°
Absorption correction: analytical Diamond anvil cell absorption correction: Absorb 6.0, R. J. Angel, J. Appl. Cryst., 2004, 37, 486-492	h = −3→3
Tmin = 0.247, Tmax = 1.000	k = −8→8
1255 measured reflections	l = −15→15
360 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.072	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.217	w = 1/[σ^2(Fo^2) + (0.1304P)^2 + 1.4756P] where P = (Fo^2 + 2Fc^2)/3
S = 0.98	(Δ/σ)max < 0.001
360 reflections	Δρmax = 0.45 e Å^−3
22 parameters	Δρmin = −0.53 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.11 (5)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

———————————————————————————— checkCIF alerts

PROBLEM: _atom_site_aniso_label is missing PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.197 Note

RESONSE: These are from a refinement against high pressure data. Many reflections have been obscured by the steel body of the pressure cell and thus not measured. There were insufficient data to allow anisotropic refinement of the atoms; all atoms were refined isotropically.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P1	0.2081 (12)	0.3022 (3)	0.13871 (16)	0.0219 (6)*
O1	0.285 (2)	0.1660 (9)	0.2524 (5)	0.0327 (12)*
O2	0.324 (2)	0.5937 (9)	0.1276 (4)	0.0295 (11)*
H2	0.3613	0.6556	0.1933	0.035*
O3	−0.073 (3)	0.3353 (11)	0.1180 (5)	0.0351 (14)*
H3	−0.1219	0.4148	0.1744	0.042*
O4	0.275 (2)	0.1373 (9)	0.0298 (4)	0.0289 (11)*
H4	0.2660	−0.0295	0.0429	0.035*

Geometric parameters (Å, º)

P1—O1	1.489 (7)	P1—O2	1.562 (7)
P1—O4	1.551 (5)	P1—O3	1.608 (17)
O1—P1—O4	113.7 (5)	O1—P1—O3	112.9 (6)
O1—P1—O2	111.8 (6)	O4—P1—O3	103.8 (6)
O4—P1—O2	105.2 (4)	O2—P1—O3	108.7 (5)

Phosphoric acid (Phosphoric_acid_II_1.8_GPa_S_Xtal)

Crystal data

H3O4P	Dx = 2.312 Mg m^−3
Mr = 97.99	Melting point: 315.5 K K
Orthorhombic, P212121	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 19 reflections
a = 4.619 (5) Å	θ = 4.8–12.4°
b = 8.479 (17) Å	µ = 0.77 mm^−1
c = 14.38 (3) Å	T = 293 K
V = 563.0 (18) Å^3	Block, colourless
Z = 8	0.2 × 0.15 × 0.08 mm
F(000) = 400

Data collection

Nonius CAD4 diffractometer	1296 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.145
Graphite monochromator	θmax = 39.6°, θmin = 2.8°
Absorption correction: analytical Diamond anvil cell absorption correction: Absorb 6.0, R. J. Angel, J. Appl. Cryst., 2004, 37, 486-492	h = −7→7
Tmin = 0.247, Tmax = 1.000	k = −9→9
2503 measured reflections	l = −22→21
1649 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.122	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.322	w = 1/[σ^2(Fo^2) + (0.0644P)^2 + 10.8552P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max < 0.001
1649 reflections	Δρmax = 1.23 e Å^−3
91 parameters	Δρmin = −1.26 e Å^−3
8 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.0 (7)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

———————————————————————————— checkCIF alerts

PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75 PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 PROBLEM: The value of Rint is greater than 0.12 PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.479 Note PROBLEM: The value of Rint is greater than 0.12 ········· 0.145 Report PROBLEM: High R1 Value ·································. 0.12 Report PROBLEM: High wR2 Value (i.e. > 0.25) ··················. 0.32 Report PROBLEM: Large Reported Max. (Positive) Residual Density 1.23 eA-3 PROBLEM: Large Reported Min. (Negative) Residual Density -1.26 eA-3 PROBLEM: s.u. on the a - Axis is (Too) Large ······ 0.005 Ang. PROBLEM: s.u. on the b - Axis is (Too) Large ······ 0.017 Ang. PROBLEM: s.u. on the c - Axis is (Too) Large ······ 0.030 Ang. PROBLEM: Short Inter D-H..H-D H13 .. H22 .. 2.12 Ang.

RESONSE: These are from a refinement against high pressure data. Many reflections have been obscured by the steel body of the pressure cell and thus not measured. Low data completeness has led to high R-factors, noisy data and large uncertainties. Short contacts are to be expected as a result of structure compression.

PROBLEM: Flack test results are meaningless. PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.8976 (6)	0.2884 (4)	−0.23095 (19)	0.0268 (7)
O11	0.6809 (16)	0.1560 (13)	−0.2046 (6)	0.038 (3)
H11	0.7241	0.1196	−0.1536	0.045*
O12	1.080 (2)	0.3361 (13)	−0.1482 (5)	0.037 (2)
O13	0.7238 (17)	0.4267 (11)	−0.2728 (6)	0.033 (2)
H13	0.6705	0.4857	−0.2309	0.040*
O14	1.073 (2)	0.2219 (15)	−0.3135 (5)	0.048 (3)
H14	1.0807	0.2881	−0.3550	0.057*
P22	0.5562 (5)	0.5113 (4)	0.0017 (2)	0.0260 (7)
O21	0.7931 (15)	0.6426 (12)	0.0140 (6)	0.031 (2)
H21	0.9446	0.6021	0.0317	0.038*
O22	0.4625 (16)	0.5321 (12)	−0.1009 (5)	0.031 (2)
H22	0.3804	0.4519	−0.1187	0.037*
O23	0.7011 (19)	0.3511 (12)	0.0174 (6)	0.035 (2)
H23	0.6020	0.2981	0.0530	0.042*
O24	0.3052 (15)	0.5377 (11)	0.0687 (5)	0.0267 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
P11	0.0254 (11)	0.028 (2)	0.0269 (13)	−0.0014 (10)	−0.0013 (10)	0.0006 (10)
O11	0.023 (3)	0.055 (9)	0.035 (5)	−0.004 (4)	−0.005 (3)	0.004 (4)
O12	0.038 (4)	0.042 (8)	0.029 (4)	−0.010 (4)	−0.007 (3)	0.003 (3)
O13	0.039 (4)	0.031 (8)	0.029 (4)	0.011 (4)	0.002 (3)	−0.001 (3)
O14	0.050 (5)	0.071 (10)	0.022 (4)	0.026 (6)	0.012 (4)	−0.005 (4)
P22	0.0216 (9)	0.028 (2)	0.0283 (12)	−0.0014 (10)	0.0011 (9)	0.0018 (10)
O21	0.016 (3)	0.029 (7)	0.050 (5)	−0.001 (3)	−0.003 (3)	0.009 (3)
O22	0.036 (4)	0.032 (7)	0.025 (4)	−0.014 (3)	−0.003 (3)	0.007 (3)
O23	0.035 (4)	0.016 (8)	0.055 (6)	0.010 (4)	0.010 (3)	0.008 (3)
O24	0.025 (3)	0.028 (7)	0.027 (4)	−0.001 (3)	0.003 (2)	−0.003 (3)

Geometric parameters (Å, º)

P11—O12	1.512 (8)	P22—O24	1.524 (7)
P11—O14	1.542 (8)	P22—O23	1.531 (9)
P11—O13	1.544 (9)	P22—O22	1.547 (8)
P11—O11	1.551 (9)	P22—O21	1.571 (8)
O12—P11—O14	114.2 (6)	O24—P22—O23	111.7 (5)
O12—P11—O13	113.1 (6)	O24—P22—O22	111.9 (5)
O14—P11—O13	104.5 (5)	O23—P22—O22	111.3 (5)
O12—P11—O11	111.2 (5)	O24—P22—O21	110.8 (5)
O14—P11—O11	105.2 (7)	O23—P22—O21	107.9 (5)
O13—P11—O11	108.0 (5)	O22—P22—O21	102.8 (5)

Phosphoric acid (Phosphoric_acid_I_0.01_GPa)

Crystal data

D3O4P	V = 321.90 (3) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.084 Mg m^−3
a = 5.7493 (5) Å	Melting point: 315.5 K K
b = 4.8392 (3) Å	Neutron radiation
c = 11.6170 (8) Å	T = 295 K
β = 95.150 (7)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.046	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1901	(Δ/σ)max = 0.01
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
54 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Negative Isotropic ADP for P ············. -0.003 Report PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of P Check

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the neutron beam is attenuated by a substantial quantity of anvil material and can cause issues with displacement parameter refinement. Refinement of the P atom Uiso to a sensible value was not possible, the only alternative being to fix it to an arbitrary positive value. Although the refined parameter is unphysical, no conclusions are being drawn from fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus of the corresponding manuscript is on molecular packing only.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.2153 (15)	0.3027 (15)	0.1388 (6)	−0.003 (2)*
O1	0.2870 (19)	0.170 (2)	0.2534 (7)	0.0080 (13)*
O2	0.3329 (19)	0.5898 (19)	0.1301 (9)	0.0080 (13)*
O3	−0.0537 (16)	0.339 (2)	0.1249 (9)	0.0080 (13)*
O4	0.291 (2)	0.1316 (18)	0.0363 (8)	0.0080 (13)*
D2	0.482 (3)	0.610 (3)	0.1758 (11)	0.041 (3)*
D3	−0.132 (3)	0.481 (2)	0.1725 (12)	0.041 (3)*
D4	0.278 (3)	−0.063 (2)	0.0478 (12)	0.041 (3)*

Geometric parameters (Å, º)

P—O1	1.502 (11)	O2—D2	0.972 (16)
P—O2	1.552 (12)	O3—D3	1.013 (16)
P—O3	1.551 (13)	O4—D4	0.955 (13)
P—O4	1.545 (12)
O1—P—O2	110.7 (7)	O3—P—O4	109.1 (7)
O1—P—O3	109.4 (7)	P—O2—D2	115.0 (12)
O1—P—O4	112.4 (7)	P—O3—D3	120.5 (13)
O2—P—O3	109.2 (7)	P—O4—D4	112.9 (12)
O2—P—O4	106.0 (7)
O1—P—O2—D2	27.9 (15)	O4—P—O3—D3	−165.6 (12)
O3—P—O2—D2	148.4 (12)	O1—P—O4—D4	37.6 (15)
O4—P—O2—D2	−94.2 (13)	O2—P—O4—D4	158.6 (12)
O1—P—O3—D3	71.1 (14)	O3—P—O4—D4	−84.0 (13)
O2—P—O3—D3	−50.2 (14)

Phosphoric acid (Phosphoric_acid_I_0.44_GPa)

Crystal data

D3O4P	V = 312.78 (2) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.145 Mg m^−3
a = 5.6927 (4) Å	Melting point: 315.5 K K
b = 4.8161 (3) Å	Neutron radiation
c = 11.4468 (7) Å	T = 295 K
β = 94.704 (6)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.051	Weighting scheme based on measured s.u.'s
R(F^2) = 0.2216	(Δ/σ)max = 0.04
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
55 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Negative Isotropic ADP for P ············. -0.006 Report PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of P Check

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the neutron beam is attenuated by a substantial quantity of anvil material and can cause issues with displacement parameter refinement. Refinement of the P atom Uiso to a sensible value was not possible, the only alternative being to fix it to an arbitrary positive value. Although the refined parameter is unphysical, no conclusions are being drawn from fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus of the corresponding manuscript is on molecular packing only.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.2102 (14)	0.3000 (13)	0.1370 (6)	−0.0059 (16)*
O1	0.2847 (17)	0.165 (2)	0.2526 (7)	0.0131 (12)*
O2	0.3194 (19)	0.5925 (17)	0.1283 (8)	0.0131 (12)*
O3	−0.0609 (16)	0.323 (2)	0.1226 (8)	0.0131 (12)*
O4	0.2824 (19)	0.1397 (17)	0.0301 (7)	0.0131 (12)*
D2	0.472 (2)	0.632 (3)	0.1733 (10)	0.044 (2)*
D3	−0.135 (2)	0.474 (2)	0.1725 (11)	0.044 (2)*
D4	0.274 (2)	−0.0628 (19)	0.0424 (11)	0.044 (2)*

Geometric parameters (Å, º)

P—O1	1.504 (11)	O2—D2	0.991 (16)
P—O2	1.546 (11)	O3—D3	1.036 (14)
P—O3	1.543 (12)	O4—D4	0.987 (12)
P—O4	1.531 (11)
O1—P—O2	111.4 (7)	O3—P—O4	106.4 (7)
O1—P—O3	109.4 (7)	P—O2—D2	118.8 (11)
O1—P—O4	114.2 (6)	P—O3—D3	116.2 (10)
O2—P—O3	109.4 (7)	P—O4—D4	111.4 (10)
O2—P—O4	105.8 (6)
O1—P—O2—D2	27.9 (14)	O4—P—O3—D3	−161.9 (10)
O3—P—O2—D2	149.0 (12)	O1—P—O4—D4	35.8 (14)
O4—P—O2—D2	−96.8 (12)	O2—P—O4—D4	158.7 (11)
O1—P—O3—D3	74.2 (12)	O3—P—O4—D4	−85.1 (12)
O2—P—O3—D3	−48.0 (12)

Phosphoric acid (Phosphoric_acid_I_0.93_GPa)

Crystal data

D3O4P	V = 304.23 (3) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.205 Mg m^−3
a = 5.6334 (4) Å	Melting point: 315.5 K K
b = 4.7900 (3) Å	Neutron radiation
c = 11.3055 (8) Å	T = 295 K
β = 94.255 (7)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.057	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1966	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
60 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of P Check

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the neutron beam is attenuated by a substantial quantity of anvil material and can cause issues with displacement parameter refinement. Refinement of the P atom Uiso to a sensible value was not possible, the only alternative being to fix it to an arbitrary positive value. Although the refined parameter is unphysical, no conclusions are being drawn from fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus of the corresponding manuscript is on molecular packing only.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.2086 (17)	0.3017 (15)	0.1349 (6)	0.000 (2)*
O1	0.291 (2)	0.169 (2)	0.2526 (9)	0.0167 (16)*
O2	0.307 (2)	0.6003 (19)	0.1272 (9)	0.0167 (16)*
O3	−0.0641 (19)	0.312 (2)	0.1223 (10)	0.0167 (16)*
O4	0.283 (2)	0.1376 (19)	0.0285 (8)	0.0167 (16)*
D2	0.465 (2)	0.638 (3)	0.1751 (12)	0.044 (2)*
D3	−0.139 (2)	0.466 (2)	0.1755 (12)	0.044 (2)*
D4	0.272 (3)	−0.068 (2)	0.0342 (12)	0.044 (2)*

Geometric parameters (Å, º)

P—O1	1.516 (12)	O2—D2	1.023 (16)
P—O2	1.539 (12)	O3—D3	1.059 (15)
P—O3	1.533 (14)	O4—D4	0.989 (13)
P—O4	1.522 (12)
O1—P—O2	110.6 (7)	O3—P—O4	106.0 (7)
O1—P—O3	109.5 (8)	P—O2—D2	115.9 (12)
O1—P—O4	113.1 (7)	P—O3—D3	114.1 (11)
O2—P—O3	109.1 (7)	P—O4—D4	116.1 (11)
O2—P—O4	108.3 (7)
O1—P—O2—D2	28.3 (15)	O4—P—O3—D3	−163.4 (11)
O3—P—O2—D2	148.8 (12)	O1—P—O4—D4	40.1 (15)
O4—P—O2—D2	−96.2 (13)	O2—P—O4—D4	163.1 (12)
O1—P—O3—D3	74.2 (12)	O3—P—O4—D4	−79.9 (13)
O2—P—O3—D3	−47.0 (13)

Phosphoric acid (Phosphoric_acid_I_1.50_GPa)

Crystal data

D3O4P	V = 295.88 (3) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.268 Mg m^−3
a = 5.5686 (4) Å	Melting point: 315.5 K K
b = 4.7647 (4) Å	Neutron radiation
c = 11.1762 (9) Å	T = 295 K
β = 93.810 (7)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.057	Weighting scheme based on measured s.u.'s
R(F^2) = 0.159	(Δ/σ)max = 0.01
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
60 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Negative Isotropic ADP for P ············. -0.005 Report PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of P Check

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the neutron beam is attenuated by a substantial quantity of anvil material and can cause issues with displacement parameter refinement. Refinement of the P atom Uiso to a sensible value was not possible, the only alternative being to fix it to an arbitrary positive value. Although the refined parameter is unphysical, no conclusions are being drawn from fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus of the corresponding manuscript is on molecular packing only.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.2036 (16)	0.3023 (14)	0.1338 (6)	−0.005 (2)*
O1	0.291 (2)	0.166 (2)	0.2511 (8)	0.0167 (16)*
O2	0.304 (2)	0.6009 (18)	0.1258 (10)	0.0167 (16)*
O3	−0.0710 (18)	0.308 (2)	0.1230 (10)	0.0167 (16)*
O4	0.278 (2)	0.144 (2)	0.0233 (8)	0.0167 (16)*
D2	0.465 (2)	0.646 (2)	0.1732 (12)	0.039 (2)*
D3	−0.149 (2)	0.459 (2)	0.1751 (11)	0.039 (2)*
D4	0.272 (2)	−0.0636 (19)	0.0272 (13)	0.039 (2)*

Geometric parameters (Å, º)

P—O1	1.514 (11)	O2—D2	1.033 (16)
P—O2	1.533 (11)	O3—D3	1.039 (15)
P—O3	1.526 (13)	O4—D4	0.991 (13)
P—O4	1.528 (12)
O1—P—O2	110.6 (7)	O3—P—O4	105.6 (7)
O1—P—O3	109.8 (8)	P—O2—D2	118.1 (10)
O1—P—O4	113.5 (7)	P—O3—D3	115.0 (10)
O2—P—O3	110.3 (7)	P—O4—D4	116.5 (11)
O2—P—O4	106.9 (7)
O1—P—O2—D2	26.8 (15)	O4—P—O3—D3	−161.4 (11)
O3—P—O2—D2	148.4 (12)	O1—P—O4—D4	39.4 (15)
O4—P—O2—D2	−97.3 (13)	O2—P—O4—D4	161.6 (12)
O1—P—O3—D3	75.8 (12)	O3—P—O4—D4	−81.0 (13)
O2—P—O3—D3	−46.2 (13)

Phosphoric acid (Phosphoric_acid_I_1.79_GPa)

Crystal data

D3O4P	V = 291.88 (3) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.299 Mg m^−3
a = 5.5356 (5) Å	Melting point: 315.5 K K
b = 4.7522 (4) Å	Neutron radiation
c = 11.1169 (9) Å	T = 295 K
β = 93.561 (8)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.058	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1683	(Δ/σ)max = 0.01
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
60 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Negative Isotropic ADP for P ············. -0.005 Report PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of P Check

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the neutron beam is attenuated by a substantial quantity of anvil material and can cause issues with displacement parameter refinement. Refinement of the P atom Uiso to a sensible value was not possible, the only alternative being to fix it to an arbitrary positive value. Although the refined parameter is unphysical, no conclusions are being drawn from fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus of the corresponding manuscript is on molecular packing only.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.2031 (16)	0.3009 (14)	0.1326 (6)	−0.005 (2)*
O1	0.289 (2)	0.162 (2)	0.2498 (8)	0.0152 (16)*
O2	0.303 (2)	0.6023 (18)	0.1286 (10)	0.0152 (16)*
O3	−0.0731 (18)	0.306 (2)	0.1238 (10)	0.0152 (16)*
O4	0.287 (2)	0.145 (2)	0.0213 (8)	0.0152 (16)*
D2	0.463 (2)	0.648 (2)	0.1712 (12)	0.039 (2)*
D3	−0.153 (2)	0.454 (2)	0.1742 (11)	0.039 (2)*
D4	0.270 (2)	−0.063 (2)	0.0241 (12)	0.039 (2)*

Geometric parameters (Å, º)

P—O1	1.511 (11)	O2—D2	1.002 (16)
P—O2	1.537 (11)	O3—D3	1.017 (15)
P—O3	1.526 (13)	O4—D4	0.994 (13)
P—O4	1.539 (12)
O1—P—O2	109.7 (7)	O3—P—O4	107.9 (7)
O1—P—O3	108.8 (7)	P—O2—D2	119.8 (10)
O1—P—O4	112.9 (7)	P—O3—D3	116.3 (11)
O2—P—O3	110.1 (7)	P—O4—D4	114.8 (11)
O2—P—O4	107.4 (7)
O1—P—O2—D2	30.7 (15)	O4—P—O3—D3	−160.3 (11)
O3—P—O2—D2	150.4 (13)	O1—P—O4—D4	44.2 (14)
O4—P—O2—D2	−92.4 (14)	O2—P—O4—D4	165.2 (12)
O1—P—O3—D3	76.9 (12)	O3—P—O4—D4	−76.1 (13)
O2—P—O3—D3	−43.4 (14)

Phosphoric acid (Phosphoric_acid_I_2.09_GPa)

Crystal data

D3O4P	V = 288.28 (3) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.327 Mg m^−3
a = 5.5049 (5) Å	Melting point: 315.5 K K
b = 4.7401 (4) Å	Neutron radiation
c = 11.0668 (10) Å	T = 295 K
β = 93.355 (9)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.064	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1481	(Δ/σ)max = 0.03
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
60 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Negative Isotropic ADP for P ············. -0.010 Report PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of P Check

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the neutron beam is attenuated by a substantial quantity of anvil material and can cause issues with displacement parameter refinement. Refinement of the P atom Uiso to a sensible value was not possible, the only alternative being to fix it to an arbitrary positive value. Although the refined parameter is unphysical, no conclusions are being drawn from fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus of the corresponding manuscript is on molecular packing only.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.2013 (16)	0.2989 (15)	0.1312 (7)	−0.0097 (14)*
O1	0.297 (2)	0.160 (2)	0.2483 (9)	0.0195 (18)*
O2	0.295 (3)	0.6052 (19)	0.1297 (11)	0.0195 (18)*
O3	−0.0769 (19)	0.300 (2)	0.1250 (11)	0.0195 (18)*
O4	0.285 (3)	0.150 (2)	0.0172 (9)	0.0195 (18)*
D2	0.462 (3)	0.652 (2)	0.1720 (13)	0.035 (2)*
D3	−0.155 (2)	0.452 (3)	0.1755 (11)	0.035 (2)*
D4	0.268 (2)	−0.058 (2)	0.0201 (12)	0.035 (2)*

Geometric parameters (Å, º)

P—O1	1.520 (13)	O2—D2	1.031 (16)
P—O2	1.541 (12)	O3—D3	1.022 (15)
P—O3	1.529 (14)	O4—D4	0.991 (13)
P—O4	1.540 (13)
O1—P—O2	108.5 (8)	O3—P—O4	108.2 (8)
O1—P—O3	109.6 (8)	P—O2—D2	119.2 (10)
O1—P—O4	113.2 (7)	P—O3—D3	115.5 (11)
O2—P—O3	109.4 (7)	P—O4—D4	113.3 (11)
O2—P—O4	107.9 (7)
O1—P—O2—D2	31.7 (16)	O4—P—O3—D3	−157.6 (11)
O3—P—O2—D2	151.3 (13)	O1—P—O4—D4	46.0 (14)
O4—P—O2—D2	−91.3 (15)	O2—P—O4—D4	166.1 (12)
O1—P—O3—D3	78.5 (13)	O3—P—O4—D4	−75.7 (13)
O2—P—O3—D3	−40.4 (14)

Phosphoric acid (Phosphoric_acid_I_2.79_GPa)

Crystal data

D3O4P	V = 280.79 (4) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.389 Mg m^−3
a = 5.4357 (6) Å	Melting point: 315.5 K K
b = 4.7148 (5) Å	Neutron radiation
c = 10.9698 (12) Å	T = 295 K
β = 92.874 (11)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.063	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1492	(Δ/σ)max = 0.01
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
60 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Negative Isotropic ADP for P ············. -0.007 Report PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of P Check

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the neutron beam is attenuated by a substantial quantity of anvil material and can cause issues with displacement parameter refinement. Refinement of the P atom Uiso to a sensible value was not possible, the only alternative being to fix it to an arbitrary positive value. Although the refined parameter is unphysical, no conclusions are being drawn from fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus of the corresponding manuscript is on molecular packing only.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.2002 (16)	0.3006 (15)	0.1290 (7)	−0.0070 (19)*
O1	0.308 (2)	0.161 (2)	0.2423 (9)	0.0147 (17)*
O2	0.289 (3)	0.6106 (18)	0.1342 (11)	0.0147 (17)*
O3	−0.0825 (19)	0.297 (2)	0.1251 (11)	0.0147 (17)*
O4	0.290 (2)	0.157 (2)	0.0113 (9)	0.0147 (17)*
D2	0.456 (3)	0.658 (2)	0.1735 (15)	0.045 (3)*
D3	−0.163 (2)	0.452 (3)	0.1769 (12)	0.045 (3)*
D4	0.273 (3)	−0.056 (2)	0.0168 (13)	0.045 (3)*

Geometric parameters (Å, º)

P—O1	1.499 (13)	O2—D2	1.01 (2)
P—O2	1.539 (11)	O3—D3	1.039 (17)
P—O3	1.535 (14)	O4—D4	1.011 (13)
P—O4	1.558 (13)
O1—P—O2	106.1 (7)	O3—P—O4	109.1 (8)
O1—P—O3	111.6 (8)	P—O2—D2	120.0 (10)
O1—P—O4	111.8 (7)	P—O3—D3	115.5 (11)
O2—P—O3	108.9 (7)	P—O4—D4	110.4 (12)
O2—P—O4	109.4 (7)
O1—P—O2—D2	32.7 (17)	O4—P—O3—D3	−155.9 (12)
O3—P—O2—D2	152.9 (15)	O1—P—O4—D4	48.0 (15)
O4—P—O2—D2	−88.0 (16)	O2—P—O4—D4	165.3 (13)
O1—P—O3—D3	80.2 (13)	O3—P—O4—D4	−75.8 (14)
O2—P—O3—D3	−36.6 (15)

Phosphoric acid (Phosphoric_acid_I_3.17_GPa)

Crystal data

D3O4P	V = 277.32 (4) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.419 Mg m^−3
a = 5.4030 (7) Å	Melting point: 315.5 K K
b = 4.7036 (6) Å	Neutron radiation
c = 10.9238 (14) Å	T = 295 K
β = 92.633 (13)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.063	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1145	(Δ/σ)max = 0.04
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
60 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Negative Isotropic ADP for P ············. -0.011 Report PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of P Check

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the neutron beam is attenuated by a substantial quantity of anvil material and can cause issues with displacement parameter refinement. Refinement of the P atom Uiso to a sensible value was not possible, the only alternative being to fix it to an arbitrary positive value. Although the refined parameter is unphysical, no conclusions are being drawn from fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus of the corresponding manuscript is on molecular packing only.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.1982 (16)	0.3010 (15)	0.1285 (7)	−0.0108 (13)*
O1	0.312 (2)	0.163 (2)	0.2410 (9)	0.0155 (18)*
O2	0.290 (3)	0.6099 (19)	0.1330 (12)	0.0155 (18)*
O3	−0.0867 (19)	0.298 (3)	0.1270 (12)	0.0155 (18)*
O4	0.291 (2)	0.159 (3)	0.0101 (9)	0.0155 (18)*
D2	0.451 (3)	0.665 (3)	0.1742 (16)	0.046 (3)*
D3	−0.167 (2)	0.450 (3)	0.1783 (13)	0.046 (3)*
D4	0.269 (3)	−0.054 (3)	0.0140 (14)	0.046 (3)*

Geometric parameters (Å, º)

P—O1	1.497 (13)	O2—D2	1.00 (2)
P—O2	1.535 (12)	O3—D3	1.018 (17)
P—O3	1.539 (13)	O4—D4	1.015 (13)
P—O4	1.559 (13)
O1—P—O2	105.3 (8)	O3—P—O4	110.3 (8)
O1—P—O3	112.2 (8)	P—O2—D2	122.4 (12)
O1—P—O4	111.1 (7)	P—O3—D3	116.1 (11)
O2—P—O3	109.3 (8)	P—O4—D4	110.3 (12)
O2—P—O4	108.4 (8)
O1—P—O2—D2	28 (2)	O4—P—O3—D3	−155.6 (13)
O3—P—O2—D2	149.0 (17)	O1—P—O4—D4	51.5 (15)
O4—P—O2—D2	−90.7 (18)	O2—P—O4—D4	166.7 (13)
O1—P—O3—D3	80.0 (14)	O3—P—O4—D4	−73.6 (14)
O2—P—O3—D3	−36.4 (16)

Phosphoric acid (Phosphoric_acid_I_0.04_GPa)

Crystal data

D3O4P	V = 321.29 (5) Å^3
Mr = 101.01	Z = 4
Monoclinic, P21/c	Cell parameters included in refinement
Hall symbol: -P 2ybc	Dx = 2.088 Mg m^−3
a = 5.7466 (8) Å	Melting point: 315.5 K K
b = 4.8378 (7) Å	Neutron radiation
c = 11.6028 (15) Å	T = 295 K
β = 95.107 (13)°	white

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	13 restraints
Rwp = 0.111	Weighting scheme based on measured s.u.'s
R(F^2) = 0.3058	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
59 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P	0.204 (2)	0.309 (3)	0.1359 (10)	0.005 (6)*
O1	0.277 (3)	0.174 (4)	0.2499 (11)	0.011 (3)*
O2	0.324 (3)	0.595 (3)	0.1322 (16)	0.011 (3)*
O3	−0.065 (2)	0.347 (4)	0.1213 (15)	0.011 (3)*
O4	0.282 (4)	0.134 (3)	0.0343 (12)	0.011 (3)*
D2	0.475 (4)	0.616 (6)	0.1741 (18)	0.038 (5)*
D3	−0.129 (4)	0.479 (4)	0.1714 (19)	0.038 (5)*
D4	0.265 (4)	−0.055 (4)	0.042 (2)	0.038 (5)*

Geometric parameters (Å, º)

P—O1	1.501 (19)	O2—D2	0.96 (3)
P—O2	1.55 (2)	O3—D3	0.96 (3)
P—O3	1.551 (17)	O4—D4	0.93 (2)
P—O4	1.55 (2)
O1—P—O2	108.9 (12)	O3—P—O4	109.6 (13)
O1—P—O3	110.2 (12)	P—O2—D2	118 (2)
O1—P—O4	110.8 (12)	P—O3—D3	116.4 (19)
O2—P—O3	109.5 (13)	P—O4—D4	115 (2)
O2—P—O4	107.9 (12)
O1—P—O2—D2	31 (3)	O4—P—O3—D3	−169 (2)
O3—P—O2—D2	152 (2)	O1—P—O4—D4	40 (3)
O4—P—O2—D2	−89 (2)	O2—P—O4—D4	160 (2)
O1—P—O3—D3	69 (2)	O3—P—O4—D4	−81 (3)
O2—P—O3—D3	−51 (2)

Phosphoric acid (Phosphoric_acid_II_0.86_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.291 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.6648 (4) Å	Neutron radiation
b = 8.6057 (7) Å	T = 295 K
c = 14.5932 (11) Å	white
V = 585.83 (5) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.043	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1366	(Δ/σ)max = 0.01
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.889 (3)	0.2929 (12)	−0.2291 (7)	0.0057 (8)*
O11	0.677 (3)	0.1643 (16)	−0.1997 (10)	0.0057 (8)*
D11	0.727 (4)	0.0831 (19)	−0.1584 (11)	0.026 (2)*
O12	1.072 (3)	0.3333 (18)	−0.1459 (9)	0.0057 (8)*
O13	0.724 (3)	0.4372 (14)	−0.2648 (10)	0.0057 (8)*
D13	0.665 (4)	0.509 (2)	−0.2187 (11)	0.026 (2)*
O14	1.077 (3)	0.2288 (17)	−0.3081 (9)	0.0057 (8)*
D14	1.154 (4)	0.297 (2)	−0.3550 (10)	0.026 (2)*
P22	0.553 (2)	0.5124 (12)	0.0012 (8)	0.0057 (8)*
O21	0.789 (3)	0.6360 (14)	0.0170 (11)	0.0057 (8)*
D21	0.979 (3)	0.602 (2)	0.0388 (13)	0.026 (2)*
O22	0.456 (3)	0.5284 (18)	−0.1003 (8)	0.0057 (8)*
D22	0.311 (4)	0.452 (2)	−0.1151 (12)	0.026 (2)*
O23	0.688 (3)	0.3494 (13)	0.0147 (11)	0.0057 (8)*
D23	0.633 (4)	0.281 (2)	0.0648 (12)	0.026 (2)*
O24	0.306 (3)	0.5313 (17)	0.0691 (9)	0.0057 (8)*

Geometric parameters (Å, º)

P11—O11	1.545 (17)	P22—O21	1.548 (16)
P11—O12	1.524 (17)	P22—O22	1.555 (17)
P11—O13	1.551 (16)	P22—O23	1.550 (16)
P11—O14	1.550 (17)	P22—O24	1.528 (17)
O11—D11	0.95 (2)	O21—D21	0.99 (2)
O13—D13	0.95 (2)	O22—D22	0.97 (2)
O14—D14	0.97 (2)	O23—D23	0.97 (2)
O11—P11—O12	107.5 (10)	O21—P22—O22	106.7 (10)
O11—P11—O13	110.4 (9)	O21—P22—O23	108.3 (9)
O11—P11—O14	108.3 (10)	O21—P22—O24	111.5 (10)
O12—P11—O13	111.3 (10)	O22—P22—O23	108.6 (10)
O12—P11—O14	110.9 (9)	O22—P22—O24	112.9 (9)
O13—P11—O14	108.4 (10)	O23—P22—O24	108.7 (10)
P11—O11—D11	123.0 (17)	P22—O21—D21	118.9 (15)
P11—O13—D13	115.1 (16)	P22—O22—D22	110.9 (15)
P11—O14—D14	121.3 (16)	P22—O23—D23	122.4 (17)
O12—P11—O11—D11	−37 (2)	O22—P22—O21—D21	−123.0 (19)
O13—P11—O11—D11	−158.7 (18)	O23—P22—O21—D21	−6 (2)
O14—P11—O11—D11	83 (2)	O24—P22—O21—D21	113.4 (19)
O11—P11—O13—D13	85.6 (19)	O21—P22—O22—D22	178.5 (16)
O12—P11—O13—D13	−34 (2)	O23—P22—O22—D22	62.0 (18)
O14—P11—O13—D13	−155.9 (17)	O24—P22—O22—D22	−58.6 (19)
O11—P11—O14—D14	150.0 (18)	O21—P22—O23—D23	113.8 (19)
O12—P11—O14—D14	−92.3 (19)	O22—P22—O23—D23	−130.7 (19)
O13—P11—O14—D14	30 (2)	O24—P22—O23—D23	−8 (2)

Phosphoric acid (Phosphoric_acid_II_1.24_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.325 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.6494 (5) Å	Neutron radiation
b = 8.5580 (9) Å	T = 295 K
c = 14.5078 (14) Å	white
V = 577.26 (6) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.045	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1263	(Δ/σ)max = 0.04
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.886 (3)	0.2884 (13)	−0.2291 (8)	0.0051 (9)*
O11	0.676 (4)	0.1572 (18)	−0.2005 (11)	0.0051 (9)*
D11	0.724 (4)	0.083 (2)	−0.1555 (12)	0.029 (2)*
O12	1.070 (4)	0.335 (2)	−0.1463 (10)	0.0051 (9)*
O13	0.724 (3)	0.4337 (15)	−0.2667 (11)	0.0051 (9)*
D13	0.664 (4)	0.511 (2)	−0.2216 (13)	0.029 (2)*
O14	1.080 (3)	0.224 (2)	−0.3074 (10)	0.0051 (9)*
D14	1.146 (5)	0.298 (2)	−0.3539 (12)	0.029 (2)*
P22	0.552 (2)	0.5108 (12)	−0.0001 (8)	0.0051 (9)*
O21	0.784 (3)	0.6384 (15)	0.0138 (11)	0.0051 (9)*
D21	0.976 (4)	0.604 (2)	0.0323 (16)	0.029 (2)*
O22	0.451 (3)	0.524 (2)	−0.1018 (9)	0.0051 (9)*
D22	0.298 (4)	0.454 (3)	−0.1185 (14)	0.029 (2)*
O23	0.688 (3)	0.3478 (14)	0.0139 (12)	0.0051 (9)*
D23	0.632 (5)	0.281 (2)	0.0649 (13)	0.029 (2)*
O24	0.307 (3)	0.5329 (18)	0.0689 (10)	0.0051 (9)*

Geometric parameters (Å, º)

P11—O11	1.55 (2)	P22—O21	1.548 (17)
P11—O12	1.53 (2)	P22—O22	1.553 (17)
P11—O13	1.553 (18)	P22—O23	1.545 (16)
P11—O14	1.552 (19)	P22—O24	1.528 (18)
O11—D11	0.94 (2)	O21—D21	0.98 (2)
O13—D13	0.97 (2)	O22—D22	0.96 (3)
O14—D14	0.98 (2)	O23—D23	0.97 (2)
O11—P11—O12	109.4 (11)	O21—P22—O22	106.5 (10)
O11—P11—O13	111.7 (12)	O21—P22—O23	109.6 (9)
O11—P11—O14	107.8 (11)	O21—P22—O24	110.3 (10)
O12—P11—O13	109.8 (11)	O22—P22—O23	108.3 (11)
O12—P11—O14	110.1 (12)	O22—P22—O24	112.8 (9)
O13—P11—O14	108.0 (11)	O23—P22—O24	109.3 (11)
P11—O11—D11	122 (2)	P22—O21—D21	117.4 (15)
P11—O13—D13	116.6 (17)	P22—O22—D22	114.7 (18)
P11—O14—D14	117.3 (18)	P22—O23—D23	121.5 (18)
O12—P11—O11—D11	−32 (2)	O22—P22—O21—D21	−120 (2)
O13—P11—O11—D11	−154 (2)	O23—P22—O21—D21	−3 (2)
O14—P11—O11—D11	88 (2)	O24—P22—O21—D21	117 (2)
O11—P11—O13—D13	87.7 (19)	O21—P22—O22—D22	−177 (2)
O12—P11—O13—D13	−34 (2)	O23—P22—O22—D22	66 (2)
O14—P11—O13—D13	−153.9 (17)	O24—P22—O22—D22	−56 (2)
O11—P11—O14—D14	148 (2)	O21—P22—O23—D23	114 (2)
O12—P11—O14—D14	−93 (2)	O22—P22—O23—D23	−130 (2)
O13—P11—O14—D14	27 (2)	O24—P22—O23—D23	−7 (2)

Phosphoric acid (Phosphoric_acid_II_1.65_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.356 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.6332 (6) Å	Neutron radiation
b = 8.5169 (10) Å	T = 295 K
c = 14.4323 (15) Å	white
V = 569.51 (7) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.045	Weighting scheme based on measured s.u.'s
R(F^2) = 0.0979	(Δ/σ)max = 0.04
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.889 (3)	0.2897 (13)	−0.2295 (8)	0.0032 (8)*
O11	0.675 (4)	0.1586 (18)	−0.2011 (11)	0.0032 (8)*
D11	0.729 (4)	0.087 (2)	−0.1558 (13)	0.028 (2)*
O12	1.072 (4)	0.3340 (19)	−0.1452 (10)	0.0032 (8)*
O13	0.723 (3)	0.4356 (15)	−0.2665 (11)	0.0032 (8)*
D13	0.651 (4)	0.513 (3)	−0.2217 (13)	0.028 (2)*
O14	1.080 (3)	0.2254 (19)	−0.3089 (10)	0.0032 (8)*
D14	1.141 (5)	0.300 (3)	−0.3551 (12)	0.028 (2)*
P22	0.556 (2)	0.5122 (12)	0.0009 (8)	0.0032 (8)*
O21	0.785 (3)	0.6428 (15)	0.0149 (11)	0.0032 (8)*
D21	0.976 (4)	0.607 (2)	0.0319 (16)	0.028 (2)*
O22	0.458 (3)	0.523 (2)	−0.1014 (9)	0.0032 (8)*
D22	0.296 (4)	0.457 (3)	−0.1191 (14)	0.028 (2)*
O23	0.696 (3)	0.3489 (14)	0.0136 (12)	0.0032 (8)*
D23	0.635 (5)	0.281 (2)	0.0644 (13)	0.028 (2)*
O24	0.302 (3)	0.5306 (17)	0.0685 (9)	0.0032 (8)*

Geometric parameters (Å, º)

P11—O11	1.55 (2)	P22—O21	1.550 (17)
P11—O12	1.53 (2)	P22—O22	1.547 (17)
P11—O13	1.556 (18)	P22—O23	1.546 (16)
P11—O14	1.548 (19)	P22—O24	1.537 (17)
O11—D11	0.93 (2)	O21—D21	0.97 (2)
O13—D13	0.98 (2)	O22—D22	0.97 (3)
O14—D14	0.96 (2)	O23—D23	0.98 (2)
O11—P11—O12	108.8 (11)	O21—P22—O22	106.4 (10)
O11—P11—O13	110.5 (12)	O21—P22—O23	110.1 (9)
O11—P11—O14	107.9 (11)	O21—P22—O24	111.6 (10)
O12—P11—O13	110.5 (11)	O22—P22—O23	106.9 (11)
O12—P11—O14	111.0 (12)	O22—P22—O24	112.0 (9)
O13—P11—O14	108.1 (11)	O23—P22—O24	109.8 (10)
P11—O11—D11	119 (2)	P22—O21—D21	115.7 (15)
P11—O13—D13	118.6 (17)	P22—O22—D22	116.3 (18)
P11—O14—D14	116.5 (18)	P22—O23—D23	120.1 (18)
O12—P11—O11—D11	−32 (2)	O22—P22—O21—D21	−118 (2)
O13—P11—O11—D11	−153 (2)	O23—P22—O21—D21	−3 (2)
O14—P11—O11—D11	89 (2)	O24—P22—O21—D21	120 (2)
O11—P11—O13—D13	84.8 (19)	O21—P22—O22—D22	−172 (2)
O12—P11—O13—D13	−36 (2)	O23—P22—O22—D22	70 (2)
O14—P11—O13—D13	−157.4 (17)	O24—P22—O22—D22	−50 (2)
O11—P11—O14—D14	146 (2)	O21—P22—O23—D23	116 (2)
O12—P11—O14—D14	−94 (2)	O22—P22—O23—D23	−129 (2)
O13—P11—O14—D14	27 (2)	O24—P22—O23—D23	−7 (2)

Phosphoric acid (Phosphoric_acid_II_1.97_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.38 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.6206 (5) Å	Neutron radiation
b = 8.4810 (9) Å	T = 295 K
c = 14.3880 (14) Å	white
V = 563.83 (6) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.039	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1002	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.891 (3)	0.2917 (13)	−0.2309 (7)	0.0041 (8)*
O11	0.676 (3)	0.1628 (17)	−0.1992 (11)	0.0041 (8)*
D11	0.731 (4)	0.084 (2)	−0.1560 (12)	0.031 (2)*
O12	1.074 (3)	0.3397 (18)	−0.1475 (10)	0.0041 (8)*
O13	0.719 (3)	0.4352 (14)	−0.2690 (10)	0.0041 (8)*
D13	0.651 (4)	0.511 (3)	−0.2240 (13)	0.031 (2)*
O14	1.080 (3)	0.2218 (18)	−0.3099 (10)	0.0041 (8)*
D14	1.145 (5)	0.297 (2)	−0.3561 (12)	0.031 (2)*
P22	0.558 (2)	0.5086 (12)	0.0016 (8)	0.0041 (8)*
O21	0.790 (3)	0.6376 (14)	0.0165 (11)	0.0041 (8)*
D21	0.981 (4)	0.603 (2)	0.0321 (16)	0.031 (2)*
O22	0.456 (3)	0.522 (2)	−0.1008 (8)	0.0041 (8)*
D22	0.299 (4)	0.456 (3)	−0.1222 (13)	0.031 (2)*
O23	0.696 (3)	0.3433 (13)	0.0129 (11)	0.0041 (8)*
D23	0.645 (4)	0.281 (2)	0.0658 (13)	0.031 (2)*
O24	0.302 (3)	0.5286 (17)	0.0692 (9)	0.0041 (8)*

Geometric parameters (Å, º)

P11—O11	1.546 (18)	P22—O21	1.547 (16)
P11—O12	1.523 (17)	P22—O22	1.551 (16)
P11—O13	1.554 (16)	P22—O23	1.549 (15)
P11—O14	1.551 (17)	P22—O24	1.541 (17)
O11—D11	0.95 (2)	O21—D21	0.96 (2)
O13—D13	0.97 (2)	O22—D22	0.97 (3)
O14—D14	0.97 (2)	O23—D23	0.96 (2)
O11—P11—O12	108.3 (10)	O21—P22—O22	106.9 (10)
O11—P11—O13	109.2 (9)	O21—P22—O23	109.9 (9)
O11—P11—O14	107.9 (10)	O21—P22—O24	111.5 (10)
O12—P11—O13	110.7 (10)	O22—P22—O23	106.9 (11)
O12—P11—O14	111.5 (9)	O22—P22—O24	111.0 (9)
O13—P11—O14	109.2 (10)	O23—P22—O24	110.5 (10)
P11—O11—D11	121.3 (17)	P22—O21—D21	117.1 (15)
P11—O13—D13	116.9 (16)	P22—O22—D22	119.2 (17)
P11—O14—D14	115.2 (17)	P22—O23—D23	118.8 (16)
O12—P11—O11—D11	−38 (2)	O22—P22—O21—D21	−118 (2)
O13—P11—O11—D11	−158.5 (19)	O23—P22—O21—D21	−2 (2)
O14—P11—O11—D11	83 (2)	O24—P22—O21—D21	121 (2)
O11—P11—O13—D13	84.2 (19)	O21—P22—O22—D22	−175 (2)
O12—P11—O13—D13	−35 (2)	O23—P22—O22—D22	67 (2)
O14—P11—O13—D13	−158.0 (17)	O24—P22—O22—D22	−53 (2)
O11—P11—O14—D14	148.8 (19)	O21—P22—O23—D23	110.4 (19)
O12—P11—O14—D14	−93 (2)	O22—P22—O23—D23	−133.9 (18)
O13—P11—O14—D14	30 (2)	O24—P22—O23—D23	−13 (2)

Phosphoric acid (Phosphoric_acid_II_2.32_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.405 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.6022 (5) Å	Neutron radiation
b = 8.4597 (9) Å	T = 295 K
c = 14.3291 (14) Å	white
V = 557.88 (6) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.041	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1086	(Δ/σ)max = 0.03
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.896 (3)	0.2904 (12)	−0.2303 (7)	0.0053 (8)*
O11	0.683 (3)	0.1592 (17)	−0.1987 (10)	0.0053 (8)*
D11	0.719 (4)	0.081 (2)	−0.1540 (12)	0.032 (2)*
O12	1.079 (3)	0.3382 (18)	−0.1469 (9)	0.0053 (8)*
O13	0.726 (3)	0.4359 (14)	−0.2681 (11)	0.0053 (8)*
D13	0.656 (4)	0.513 (2)	−0.2230 (13)	0.032 (2)*
O14	1.085 (3)	0.2203 (18)	−0.3095 (9)	0.0053 (8)*
D14	1.136 (5)	0.293 (2)	−0.3587 (12)	0.032 (2)*
P22	0.555 (2)	0.5110 (12)	−0.0010 (8)	0.0053 (8)*
O21	0.789 (3)	0.6402 (15)	0.0134 (11)	0.0053 (8)*
D21	0.977 (4)	0.604 (2)	0.0325 (15)	0.032 (2)*
O22	0.459 (3)	0.524 (2)	−0.1042 (9)	0.0053 (8)*
D22	0.287 (4)	0.466 (3)	−0.1203 (13)	0.032 (2)*
O23	0.693 (3)	0.3452 (14)	0.0112 (11)	0.0053 (8)*
D23	0.646 (4)	0.282 (2)	0.0657 (13)	0.032 (2)*
O24	0.300 (3)	0.5329 (16)	0.0667 (9)	0.0053 (8)*

Geometric parameters (Å, º)

P11—O11	1.549 (18)	P22—O21	1.548 (17)
P11—O12	1.517 (18)	P22—O22	1.547 (17)
P11—O13	1.556 (17)	P22—O23	1.550 (16)
P11—O14	1.548 (18)	P22—O24	1.534 (17)
O11—D11	0.94 (2)	O21—D21	0.96 (2)
O13—D13	0.97 (2)	O22—D22	0.96 (3)
O14—D14	0.97 (2)	O23—D23	0.97 (2)
O11—P11—O12	108.2 (10)	O21—P22—O22	106.0 (10)
O11—P11—O13	110.5 (11)	O21—P22—O23	109.8 (9)
O11—P11—O14	107.2 (10)	O21—P22—O24	111.3 (10)
O12—P11—O13	110.0 (10)	O22—P22—O23	106.8 (11)
O12—P11—O14	111.6 (11)	O22—P22—O24	112.2 (9)
O13—P11—O14	109.3 (10)	O23—P22—O24	110.6 (10)
P11—O11—D11	126.5 (17)	P22—O21—D21	116.2 (15)
P11—O13—D13	117.8 (17)	P22—O22—D22	115.4 (17)
P11—O14—D14	115.4 (17)	P22—O23—D23	119.9 (16)
O12—P11—O11—D11	−34 (2)	O22—P22—O21—D21	−120 (2)
O13—P11—O11—D11	−154 (2)	O23—P22—O21—D21	−5 (2)
O14—P11—O11—D11	87 (2)	O24—P22—O21—D21	118 (2)
O11—P11—O13—D13	84.0 (19)	O21—P22—O22—D22	−168 (2)
O12—P11—O13—D13	−35 (2)	O23—P22—O22—D22	75 (2)
O14—P11—O13—D13	−158.3 (17)	O24—P22—O22—D22	−46 (2)
O11—P11—O14—D14	144.0 (19)	O21—P22—O23—D23	109.2 (19)
O12—P11—O14—D14	−98 (2)	O22—P22—O23—D23	−136.3 (18)
O13—P11—O14—D14	24 (2)	O24—P22—O23—D23	−14 (2)

Phosphoric acid (Phosphoric_acid_II_2.45_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.417 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5980 (6) Å	Neutron radiation
b = 8.4429 (10) Å	T = 295 K
c = 14.3036 (16) Å	white
V = 555.27 (7) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.047	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1559	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.891 (3)	0.2897 (13)	−0.2305 (8)	0.0047 (10)*
O11	0.672 (4)	0.1609 (18)	−0.1997 (12)	0.0047 (10)*
D11	0.727 (5)	0.084 (2)	−0.1541 (14)	0.032 (3)*
O12	1.075 (4)	0.338 (2)	−0.1469 (11)	0.0047 (10)*
O13	0.726 (4)	0.4362 (16)	−0.2690 (12)	0.0047 (10)*
D13	0.656 (5)	0.522 (3)	−0.2304 (16)	0.032 (3)*
O14	1.083 (4)	0.218 (2)	−0.3088 (10)	0.0047 (10)*
D14	1.126 (6)	0.288 (3)	−0.3593 (14)	0.032 (3)*
P22	0.562 (2)	0.5078 (13)	0.0008 (9)	0.0047 (10)*
O21	0.798 (3)	0.6357 (16)	0.0166 (13)	0.0047 (10)*
D21	0.993 (4)	0.611 (3)	0.0348 (18)	0.032 (3)*
O22	0.462 (3)	0.523 (2)	−0.1022 (9)	0.0047 (10)*
D22	0.284 (4)	0.471 (3)	−0.1181 (15)	0.032 (3)*
O23	0.697 (4)	0.3411 (14)	0.0147 (12)	0.0047 (10)*
D23	0.653 (5)	0.280 (2)	0.0688 (14)	0.032 (3)*
O24	0.308 (3)	0.5312 (18)	0.0681 (10)	0.0047 (10)*

Geometric parameters (Å, º)

P11—O11	1.55 (2)	P22—O21	1.548 (17)
P11—O12	1.52 (2)	P22—O22	1.549 (18)
P11—O13	1.552 (19)	P22—O23	1.551 (17)
P11—O14	1.55 (2)	P22—O24	1.526 (18)
O11—D11	0.95 (3)	O21—D21	0.96 (2)
O13—D13	0.97 (3)	O22—D22	0.96 (2)
O14—D14	0.95 (2)	O23—D23	0.95 (2)
O11—P11—O12	109.1 (11)	O21—P22—O22	106.8 (11)
O11—P11—O13	110.1 (12)	O21—P22—O23	109.5 (10)
O11—P11—O14	107.6 (11)	O21—P22—O24	110.7 (11)
O12—P11—O13	109.7 (11)	O22—P22—O23	108.4 (11)
O12—P11—O14	110.9 (12)	O22—P22—O24	111.2 (9)
O13—P11—O14	109.5 (11)	O23—P22—O24	110.1 (11)
P11—O11—D11	120 (2)	P22—O21—D21	123.0 (16)
P11—O13—D13	124 (2)	P22—O22—D22	116.3 (18)
P11—O14—D14	115.1 (19)	P22—O23—D23	120.7 (19)
O12—P11—O11—D11	−36 (2)	O22—P22—O21—D21	−120 (3)
O13—P11—O11—D11	−156 (2)	O23—P22—O21—D21	−3 (3)
O14—P11—O11—D11	85 (2)	O24—P22—O21—D21	119 (3)
O11—P11—O13—D13	87 (3)	O21—P22—O22—D22	−165 (2)
O12—P11—O13—D13	−33 (3)	O23—P22—O22—D22	78 (2)
O14—P11—O13—D13	−155 (2)	O24—P22—O22—D22	−44 (2)
O11—P11—O14—D14	140 (2)	O21—P22—O23—D23	107 (2)
O12—P11—O14—D14	−101 (2)	O22—P22—O23—D23	−137 (2)
O13—P11—O14—D14	20 (3)	O24—P22—O23—D23	−15 (3)

Phosphoric acid (Phosphoric_acid_II_2.63_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.426 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5932 (5) Å	Neutron radiation
b = 8.4323 (8) Å	T = 295 K
c = 14.2795 (13) Å	white
V = 553.06 (6) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.040	Weighting scheme based on measured s.u.'s
R(F^2) = 0.0949	(Δ/σ)max = 0.05
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.894 (2)	0.2905 (12)	−0.2318 (7)	0.0031 (7)*
O11	0.676 (3)	0.1619 (16)	−0.1997 (10)	0.0031 (7)*
D11	0.721 (4)	0.082 (2)	−0.1551 (11)	0.031 (2)*
O12	1.085 (3)	0.3357 (17)	−0.1477 (9)	0.0031 (7)*
O13	0.727 (3)	0.4377 (14)	−0.2700 (10)	0.0031 (7)*
D13	0.649 (4)	0.510 (2)	−0.2244 (12)	0.031 (2)*
O14	1.075 (3)	0.2164 (17)	−0.3124 (9)	0.0031 (7)*
D14	1.141 (5)	0.294 (2)	−0.3570 (11)	0.031 (2)*
P22	0.561 (2)	0.5076 (12)	0.0021 (7)	0.0031 (7)*
O21	0.795 (3)	0.6370 (14)	0.0182 (11)	0.0031 (7)*
D21	0.987 (4)	0.606 (2)	0.0356 (14)	0.031 (2)*
O22	0.461 (3)	0.5238 (18)	−0.1012 (8)	0.0031 (7)*
D22	0.288 (4)	0.467 (3)	−0.1207 (12)	0.031 (2)*
O23	0.700 (3)	0.3411 (13)	0.0136 (10)	0.0031 (7)*
D23	0.642 (4)	0.279 (2)	0.0677 (12)	0.031 (2)*
O24	0.302 (3)	0.5273 (16)	0.0699 (9)	0.0031 (7)*

Geometric parameters (Å, º)

P11—O11	1.546 (17)	P22—O21	1.549 (16)
P11—O12	1.535 (16)	P22—O22	1.551 (15)
P11—O13	1.558 (16)	P22—O23	1.551 (15)
P11—O14	1.551 (17)	P22—O24	1.543 (16)
O11—D11	0.95 (2)	O21—D21	0.95 (2)
O13—D13	0.96 (2)	O22—D22	0.97 (2)
O14—D14	0.96 (2)	O23—D23	0.97 (2)
O11—P11—O12	108.2 (10)	O21—P22—O22	106.5 (10)
O11—P11—O13	110.1 (9)	O21—P22—O23	109.7 (9)
O11—P11—O14	106.5 (9)	O21—P22—O24	111.5 (10)
O12—P11—O13	111.0 (10)	O22—P22—O23	107.6 (10)
O12—P11—O14	112.0 (9)	O22—P22—O24	111.0 (9)
O13—P11—O14	109.0 (9)	O23—P22—O24	110.4 (9)
P11—O11—D11	123.8 (17)	P22—O21—D21	119.2 (15)
P11—O13—D13	116.9 (16)	P22—O22—D22	118.2 (16)
P11—O14—D14	112.7 (16)	P22—O23—D23	117.4 (16)
O12—P11—O11—D11	−35 (2)	O22—P22—O21—D21	−119 (2)
O13—P11—O11—D11	−156.5 (18)	O23—P22—O21—D21	−3 (2)
O14—P11—O11—D11	86 (2)	O24—P22—O21—D21	120 (2)
O11—P11—O13—D13	79.5 (19)	O21—P22—O22—D22	−168 (2)
O12—P11—O13—D13	−40 (2)	O23—P22—O22—D22	75 (2)
O14—P11—O13—D13	−164.0 (17)	O24—P22—O22—D22	−46 (2)
O11—P11—O14—D14	150.3 (18)	O21—P22—O23—D23	110.9 (18)
O12—P11—O14—D14	−91.6 (19)	O22—P22—O23—D23	−133.7 (17)
O13—P11—O14—D14	32 (2)	O24—P22—O23—D23	−12 (2)

Phosphoric acid (Phosphoric_acid_II_2.78_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.435 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5868 (7) Å	Neutron radiation
b = 8.4232 (13) Å	T = 295 K
c = 14.2653 (19) Å	white
V = 551.15 (8) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.055	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1234	(Δ/σ)max = 0.03
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.892 (3)	0.2890 (15)	−0.2303 (8)	0.0037 (11)*
O11	0.670 (4)	0.161 (2)	−0.1987 (13)	0.0037 (11)*
D11	0.720 (6)	0.081 (3)	−0.1542 (15)	0.029 (3)*
O12	1.083 (4)	0.334 (2)	−0.1478 (11)	0.0037 (11)*
O13	0.726 (4)	0.4378 (18)	−0.2663 (13)	0.0037 (11)*
D13	0.656 (5)	0.518 (3)	−0.2242 (17)	0.029 (3)*
O14	1.079 (4)	0.218 (2)	−0.3105 (11)	0.0037 (11)*
D14	1.137 (6)	0.288 (3)	−0.3602 (15)	0.029 (3)*
P22	0.560 (3)	0.5103 (14)	−0.0006 (9)	0.0037 (11)*
O21	0.790 (3)	0.6406 (18)	0.0187 (15)	0.0037 (11)*
D21	0.987 (4)	0.609 (3)	0.032 (2)	0.029 (3)*
O22	0.463 (4)	0.525 (3)	−0.1043 (10)	0.0037 (11)*
D22	0.295 (5)	0.466 (4)	−0.1217 (17)	0.029 (3)*
O23	0.700 (4)	0.3447 (16)	0.0141 (14)	0.0037 (11)*
D23	0.647 (6)	0.280 (3)	0.0663 (16)	0.029 (3)*
O24	0.302 (4)	0.530 (2)	0.0649 (11)	0.0037 (11)*

Geometric parameters (Å, º)

P11—O11	1.55 (2)	P22—O21	1.55 (2)
P11—O12	1.52 (2)	P22—O22	1.55 (2)
P11—O13	1.55 (2)	P22—O23	1.550 (19)
P11—O14	1.55 (2)	P22—O24	1.52 (2)
O11—D11	0.95 (3)	O21—D21	0.96 (2)
O13—D13	0.96 (3)	O22—D22	0.95 (3)
O14—D14	0.96 (3)	O23—D23	0.95 (3)
O11—P11—O12	109.1 (12)	O21—P22—O22	108.0 (13)
O11—P11—O13	109.6 (12)	O21—P22—O23	109.4 (12)
O11—P11—O14	108.1 (12)	O21—P22—O24	110.2 (12)
O12—P11—O13	109.8 (12)	O22—P22—O23	108.7 (12)
O12—P11—O14	110.5 (13)	O22—P22—O24	110.8 (12)
O13—P11—O14	109.8 (12)	O23—P22—O24	109.8 (12)
P11—O11—D11	122 (2)	P22—O21—D21	119 (2)
P11—O13—D13	122 (2)	P22—O22—D22	116 (2)
P11—O14—D14	118 (2)	P22—O23—D23	121 (2)
O12—P11—O11—D11	−36 (3)	O22—P22—O21—D21	−114 (3)
O13—P11—O11—D11	−156 (2)	O23—P22—O21—D21	5 (3)
O14—P11—O11—D11	85 (3)	O24—P22—O21—D21	125 (3)
O11—P11—O13—D13	84 (3)	O21—P22—O22—D22	−168 (3)
O12—P11—O13—D13	−36 (3)	O23—P22—O22—D22	74 (3)
O14—P11—O13—D13	−158 (2)	O24—P22—O22—D22	−47 (3)
O11—P11—O14—D14	144 (2)	O21—P22—O23—D23	109 (3)
O12—P11—O14—D14	−97 (2)	O22—P22—O23—D23	−133 (3)
O13—P11—O14—D14	24 (3)	O24—P22—O23—D23	−12 (3)

Phosphoric acid (Phosphoric_acid_II_2.91_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.444 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5831 (5) Å	Neutron radiation
b = 8.4110 (9) Å	T = 295 K
c = 14.2424 (14) Å	white
V = 549.02 (6) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.040	Weighting scheme based on measured s.u.'s
R(F^2) = 0.0952	(Δ/σ)max = 0.03
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.893 (3)	0.2892 (12)	−0.2305 (7)	0.0031 (8)*
O11	0.672 (3)	0.1608 (17)	−0.1990 (10)	0.0031 (8)*
D11	0.726 (4)	0.082 (2)	−0.1546 (12)	0.028 (2)*
O12	1.076 (3)	0.3384 (18)	−0.1460 (9)	0.0031 (8)*
O13	0.725 (3)	0.4364 (15)	−0.2688 (11)	0.0031 (8)*
D13	0.660 (4)	0.518 (2)	−0.2251 (13)	0.028 (2)*
O14	1.086 (3)	0.2174 (18)	−0.3091 (9)	0.0031 (8)*
D14	1.130 (5)	0.291 (2)	−0.3585 (12)	0.028 (2)*
P22	0.560 (2)	0.5104 (12)	−0.0021 (8)	0.0031 (8)*
O21	0.794 (3)	0.6410 (14)	0.0119 (11)	0.0031 (8)*
D21	0.981 (4)	0.609 (2)	0.0339 (15)	0.028 (2)*
O22	0.463 (3)	0.524 (2)	−0.1059 (9)	0.0031 (8)*
D22	0.289 (4)	0.468 (3)	−0.1207 (13)	0.028 (2)*
O23	0.702 (3)	0.3453 (14)	0.0123 (11)	0.0031 (8)*
D23	0.649 (4)	0.281 (2)	0.0669 (13)	0.028 (2)*
O24	0.298 (3)	0.5298 (16)	0.0660 (9)	0.0031 (8)*

Geometric parameters (Å, º)

P11—O11	1.547 (17)	P22—O21	1.548 (16)
P11—O12	1.524 (17)	P22—O22	1.548 (17)
P11—O13	1.557 (17)	P22—O23	1.547 (16)
P11—O14	1.549 (17)	P22—O24	1.552 (17)
O11—D11	0.95 (2)	O21—D21	0.95 (2)
O13—D13	0.97 (2)	O22—D22	0.95 (2)
O14—D14	0.96 (2)	O23—D23	0.98 (2)
O11—P11—O12	108.7 (10)	O21—P22—O22	105.6 (10)
O11—P11—O13	109.5 (9)	O21—P22—O23	109.2 (9)
O11—P11—O14	108.1 (10)	O21—P22—O24	112.4 (10)
O12—P11—O13	109.5 (10)	O22—P22—O23	108.3 (11)
O12—P11—O14	111.2 (9)	O22—P22—O24	111.5 (9)
O13—P11—O14	109.8 (10)	O23—P22—O24	109.7 (10)
P11—O11—D11	120.7 (16)	P22—O21—D21	117.8 (15)
P11—O13—D13	119.2 (17)	P22—O22—D22	114.6 (17)
P11—O14—D14	113.5 (17)	P22—O23—D23	119.8 (16)
O12—P11—O11—D11	−38 (2)	O22—P22—O21—D21	−123 (2)
O13—P11—O11—D11	−157.3 (18)	O23—P22—O21—D21	−7 (2)
O14—P11—O11—D11	83 (2)	O24—P22—O21—D21	115 (2)
O11—P11—O13—D13	86.1 (19)	O21—P22—O22—D22	−166 (2)
O12—P11—O13—D13	−33 (2)	O23—P22—O22—D22	77 (2)
O14—P11—O13—D13	−155.3 (17)	O24—P22—O22—D22	−44 (2)
O11—P11—O14—D14	141.0 (18)	O21—P22—O23—D23	111.4 (19)
O12—P11—O14—D14	−99.7 (19)	O22—P22—O23—D23	−134.1 (18)
O13—P11—O14—D14	22 (2)	O24—P22—O23—D23	−12 (2)

Phosphoric acid (Phosphoric_acid_II_3.04_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.452 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5791 (8) Å	Neutron radiation
b = 8.4031 (14) Å	T = 295 K
c = 14.221 (2) Å	white
V = 547.22 (9) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.058	Weighting scheme based on measured s.u.'s
R(F^2) = 0.156	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.888 (3)	0.2908 (16)	−0.2316 (10)	0.0063 (13)*
O11	0.666 (4)	0.164 (2)	−0.1977 (15)	0.0063 (13)*
D11	0.725 (6)	0.086 (3)	−0.1531 (18)	0.035 (3)*
O12	1.078 (5)	0.339 (3)	−0.1496 (13)	0.0063 (13)*
O13	0.726 (5)	0.439 (2)	−0.2709 (15)	0.0063 (13)*
D13	0.642 (6)	0.508 (4)	−0.2257 (18)	0.035 (3)*
O14	1.076 (4)	0.218 (3)	−0.3110 (13)	0.0063 (13)*
D14	1.124 (7)	0.294 (3)	−0.3591 (17)	0.035 (3)*
P22	0.563 (3)	0.5112 (15)	0.0001 (10)	0.0063 (13)*
O21	0.788 (4)	0.646 (2)	0.0150 (16)	0.0063 (13)*
D21	0.973 (5)	0.602 (3)	0.033 (2)	0.035 (3)*
O22	0.463 (4)	0.520 (3)	−0.1038 (11)	0.0063 (13)*
D22	0.292 (6)	0.462 (4)	−0.1205 (19)	0.035 (3)*
O23	0.711 (4)	0.3476 (18)	0.0164 (16)	0.0063 (13)*
D23	0.656 (6)	0.276 (3)	0.0662 (18)	0.035 (3)*
O24	0.304 (4)	0.532 (2)	0.0669 (13)	0.0063 (13)*

Geometric parameters (Å, º)

P11—O11	1.55 (2)	P22—O21	1.55 (2)
P11—O12	1.51 (3)	P22—O22	1.55 (2)
P11—O13	1.55 (2)	P22—O23	1.55 (2)
P11—O14	1.55 (2)	P22—O24	1.53 (2)
O11—D11	0.95 (3)	O21—D21	0.96 (3)
O13—D13	0.95 (4)	O22—D22	0.95 (4)
O14—D14	0.96 (3)	O23—D23	0.96 (3)
O11—P11—O12	108.8 (14)	O21—P22—O22	107.0 (14)
O11—P11—O13	110.5 (13)	O21—P22—O23	109.8 (13)
O11—P11—O14	108.7 (13)	O21—P22—O24	110.4 (13)
O12—P11—O13	109.8 (15)	O22—P22—O23	108.3 (15)
O12—P11—O14	110.4 (14)	O22—P22—O24	111.0 (13)
O13—P11—O14	108.7 (13)	O23—P22—O24	110.3 (13)
P11—O11—D11	120 (2)	P22—O21—D21	110 (2)
P11—O13—D13	116 (3)	P22—O22—D22	117 (2)
P11—O14—D14	113 (2)	P22—O23—D23	123 (2)
O12—P11—O11—D11	−37 (3)	O22—P22—O21—D21	−119 (3)
O13—P11—O11—D11	−158 (3)	O23—P22—O21—D21	−2 (3)
O14—P11—O11—D11	83 (3)	O24—P22—O21—D21	120 (3)
O11—P11—O13—D13	76 (3)	O21—P22—O22—D22	−166 (3)
O12—P11—O13—D13	−45 (3)	O23—P22—O22—D22	76 (3)
O14—P11—O13—D13	−165 (3)	O24—P22—O22—D22	−45 (3)
O11—P11—O14—D14	144 (2)	O21—P22—O23—D23	116 (3)
O12—P11—O14—D14	−97 (3)	O22—P22—O23—D23	−127 (3)
O13—P11—O14—D14	23 (3)	O24—P22—O23—D23	−6 (3)

Phosphoric acid (Phosphoric_acid_II_3.42_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.474 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5689 (7) Å	Neutron radiation
b = 8.3733 (12) Å	T = 295 K
c = 14.1755 (18) Å	white
V = 542.32 (8) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.050	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1236	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.883 (3)	0.2857 (14)	−0.2325 (8)	0.0031 (10)*
O11	0.661 (4)	0.1572 (19)	−0.2001 (12)	0.0031 (10)*
D11	0.720 (6)	0.085 (3)	−0.1521 (16)	0.036 (3)*
O12	1.072 (4)	0.336 (2)	−0.1497 (11)	0.0031 (10)*
O13	0.717 (4)	0.4330 (17)	−0.2721 (13)	0.0031 (10)*
D13	0.662 (5)	0.514 (3)	−0.2277 (17)	0.036 (3)*
O14	1.073 (4)	0.211 (2)	−0.3116 (11)	0.0031 (10)*
D14	1.133 (6)	0.291 (3)	−0.3557 (16)	0.036 (3)*
P22	0.561 (3)	0.5093 (13)	0.0006 (9)	0.0031 (10)*
O21	0.790 (3)	0.6430 (17)	0.0170 (14)	0.0031 (10)*
D21	0.984 (4)	0.609 (3)	0.035 (2)	0.036 (3)*
O22	0.460 (4)	0.524 (2)	−0.1033 (9)	0.0031 (10)*
D22	0.285 (5)	0.466 (4)	−0.1187 (17)	0.036 (3)*
O23	0.707 (4)	0.3436 (15)	0.0142 (13)	0.0031 (10)*
D23	0.639 (5)	0.278 (3)	0.0658 (16)	0.036 (3)*
O24	0.302 (3)	0.5272 (19)	0.0667 (11)	0.0031 (10)*

Geometric parameters (Å, º)

P11—O11	1.55 (2)	P22—O21	1.550 (19)
P11—O12	1.52 (2)	P22—O22	1.548 (19)
P11—O13	1.55 (2)	P22—O23	1.552 (18)
P11—O14	1.55 (2)	P22—O24	1.52 (2)
O11—D11	0.95 (3)	O21—D21	0.97 (2)
O13—D13	0.96 (3)	O22—D22	0.96 (3)
O14—D14	0.96 (3)	O23—D23	0.97 (3)
O11—P11—O12	109.7 (11)	O21—P22—O22	106.7 (12)
O11—P11—O13	109.8 (12)	O21—P22—O23	109.7 (12)
O11—P11—O14	107.5 (11)	O21—P22—O24	111.3 (11)
O12—P11—O13	109.7 (11)	O22—P22—O23	108.5 (12)
O12—P11—O14	110.7 (12)	O22—P22—O24	110.3 (12)
O13—P11—O14	109.4 (11)	O23—P22—O24	110.3 (12)
P11—O11—D11	118 (2)	P22—O21—D21	116.5 (19)
P11—O13—D13	117 (2)	P22—O22—D22	115 (2)
P11—O14—D14	111 (2)	P22—O23—D23	118 (2)
O12—P11—O11—D11	−33 (3)	O22—P22—O21—D21	−119 (3)
O13—P11—O11—D11	−154 (2)	O23—P22—O21—D21	−2 (3)
O14—P11—O11—D11	87 (2)	O24—P22—O21—D21	120 (3)
O11—P11—O13—D13	88 (2)	O21—P22—O22—D22	−165 (2)
O12—P11—O13—D13	−33 (3)	O23—P22—O22—D22	77 (3)
O14—P11—O13—D13	−154 (2)	O24—P22—O22—D22	−45 (3)
O11—P11—O14—D14	149 (2)	O21—P22—O23—D23	115 (2)
O12—P11—O14—D14	−92 (2)	O22—P22—O23—D23	−128 (2)
O13—P11—O14—D14	29 (3)	O24—P22—O23—D23	−8 (3)

Phosphoric acid (Phosphoric_acid_II_3.60_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.485 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5639 (6) Å	Neutron radiation
b = 8.3606 (10) Å	T = 295 K
c = 14.1535 (15) Å	white
V = 540.05 (7) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.040	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1029	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.886 (3)	0.2900 (13)	−0.2314 (8)	0.0021 (8)*
O11	0.664 (3)	0.1609 (17)	−0.2001 (11)	0.0021 (8)*
D11	0.716 (5)	0.083 (2)	−0.1533 (14)	0.032 (2)*
O12	1.075 (3)	0.3400 (18)	−0.1471 (10)	0.0021 (8)*
O13	0.723 (3)	0.4372 (15)	−0.2726 (11)	0.0021 (8)*
D13	0.647 (4)	0.509 (3)	−0.2272 (14)	0.032 (2)*
O14	1.076 (3)	0.2155 (19)	−0.3107 (10)	0.0021 (8)*
D14	1.134 (5)	0.292 (3)	−0.3582 (13)	0.032 (2)*
P22	0.564 (2)	0.5104 (12)	−0.0015 (8)	0.0021 (8)*
O21	0.802 (3)	0.6395 (15)	0.0147 (12)	0.0021 (8)*
D21	0.996 (4)	0.609 (2)	0.0372 (16)	0.032 (2)*
O22	0.461 (3)	0.5289 (19)	−0.1052 (9)	0.0021 (8)*
D22	0.285 (4)	0.471 (3)	−0.1209 (14)	0.032 (2)*
O23	0.707 (3)	0.3436 (14)	0.0114 (11)	0.0021 (8)*
D23	0.640 (4)	0.279 (2)	0.0652 (14)	0.032 (2)*
O24	0.299 (3)	0.5279 (16)	0.0659 (9)	0.0021 (8)*

Geometric parameters (Å, º)

P11—O11	1.545 (17)	P22—O21	1.548 (16)
P11—O12	1.531 (18)	P22—O22	1.549 (17)
P11—O13	1.552 (17)	P22—O23	1.551 (16)
P11—O14	1.549 (18)	P22—O24	1.547 (17)
O11—D11	0.96 (2)	O21—D21	0.98 (2)
O13—D13	0.95 (3)	O22—D22	0.96 (2)
O14—D14	0.97 (2)	O23—D23	0.98 (2)
O11—P11—O12	109.7 (10)	O21—P22—O22	106.5 (10)
O11—P11—O13	110.3 (9)	O21—P22—O23	108.3 (9)
O11—P11—O14	107.1 (10)	O21—P22—O24	113.0 (10)
O12—P11—O13	110.3 (10)	O22—P22—O23	109.2 (10)
O12—P11—O14	111.1 (9)	O22—P22—O24	109.7 (9)
O13—P11—O14	108.4 (10)	O23—P22—O24	110.0 (10)
P11—O11—D11	120.7 (18)	P22—O21—D21	120.2 (15)
P11—O13—D13	115.1 (19)	P22—O22—D22	114.9 (17)
P11—O14—D14	113.1 (17)	P22—O23—D23	117.1 (16)
O12—P11—O11—D11	−35 (2)	O22—P22—O21—D21	−124 (2)
O13—P11—O11—D11	−156.5 (19)	O23—P22—O21—D21	−7 (2)
O14—P11—O11—D11	86 (2)	O24—P22—O21—D21	115 (2)
O11—P11—O13—D13	81 (2)	O21—P22—O22—D22	−168 (2)
O12—P11—O13—D13	−41 (2)	O23—P22—O22—D22	76 (2)
O14—P11—O13—D13	−162.5 (18)	O24—P22—O22—D22	−45 (2)
O11—P11—O14—D14	145.8 (18)	O21—P22—O23—D23	114.0 (18)
O12—P11—O14—D14	−95 (2)	O22—P22—O23—D23	−130.4 (18)
O13—P11—O14—D14	27 (2)	O24—P22—O23—D23	−10 (2)

Phosphoric acid (Phosphoric_acid_II_3.74_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.494 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5599 (9) Å	Neutron radiation
b = 8.3496 (15) Å	T = 295 K
c = 14.133 (2) Å	white
V = 538.10 (10) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.060	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1292	(Δ/σ)max = 0.03
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.885 (3)	0.2873 (16)	−0.2335 (9)	0.0025 (12)*
O11	0.667 (4)	0.156 (2)	−0.2008 (14)	0.0025 (12)*
D11	0.699 (8)	0.083 (4)	−0.1498 (19)	0.050 (4)*
O12	1.072 (4)	0.340 (3)	−0.1507 (12)	0.0025 (12)*
O13	0.715 (4)	0.4340 (19)	−0.2727 (15)	0.0025 (12)*
D13	0.642 (6)	0.507 (4)	−0.227 (2)	0.050 (4)*
O14	1.078 (4)	0.216 (3)	−0.3131 (12)	0.0025 (12)*
D14	1.124 (8)	0.295 (4)	−0.360 (2)	0.050 (4)*
P22	0.564 (3)	0.5081 (15)	0.0000 (10)	0.0025 (12)*
O21	0.791 (4)	0.642 (2)	0.0200 (16)	0.0025 (12)*
D21	0.985 (5)	0.606 (4)	0.035 (3)	0.050 (4)*
O22	0.459 (4)	0.524 (3)	−0.1038 (11)	0.0025 (12)*
D22	0.281 (6)	0.472 (5)	−0.121 (2)	0.050 (4)*
O23	0.712 (4)	0.3426 (18)	0.0130 (15)	0.0025 (12)*
D23	0.661 (7)	0.278 (4)	0.0663 (19)	0.050 (4)*
O24	0.304 (4)	0.523 (2)	0.0672 (12)	0.0025 (12)*

Geometric parameters (Å, º)

P11—O11	1.55 (2)	P22—O21	1.55 (2)
P11—O12	1.51 (2)	P22—O22	1.55 (2)
P11—O13	1.55 (2)	P22—O23	1.55 (2)
P11—O14	1.55 (2)	P22—O24	1.52 (2)
O11—D11	0.96 (4)	O21—D21	0.96 (3)
O13—D13	0.95 (4)	O22—D22	0.95 (4)
O14—D14	0.96 (4)	O23—D23	0.96 (3)
O11—P11—O12	109.7 (12)	O21—P22—O22	108.5 (14)
O11—P11—O13	110.1 (12)	O21—P22—O23	109.3 (12)
O11—P11—O14	108.0 (12)	O21—P22—O24	110.3 (13)
O12—P11—O13	109.2 (12)	O22—P22—O23	108.9 (14)
O12—P11—O14	110.7 (13)	O22—P22—O24	110.0 (13)
O13—P11—O14	109.2 (13)	O23—P22—O24	109.8 (13)
P11—O11—D11	125 (3)	P22—O21—D21	116 (2)
P11—O13—D13	116 (3)	P22—O22—D22	118 (2)
P11—O14—D14	111 (2)	P22—O23—D23	119 (3)
O12—P11—O11—D11	−28 (3)	O22—P22—O21—D21	−117 (3)
O13—P11—O11—D11	−148 (3)	O23—P22—O21—D21	2 (4)
O14—P11—O11—D11	93 (3)	O24—P22—O21—D21	123 (3)
O11—P11—O13—D13	82 (3)	O21—P22—O22—D22	−162 (3)
O12—P11—O13—D13	−39 (3)	O23—P22—O22—D22	79 (3)
O14—P11—O13—D13	−160 (2)	O24—P22—O22—D22	−41 (4)
O11—P11—O14—D14	145 (3)	O21—P22—O23—D23	109 (3)
O12—P11—O14—D14	−96 (3)	O22—P22—O23—D23	−133 (3)
O13—P11—O14—D14	25 (3)	O24—P22—O23—D23	−12 (3)

Phosphoric acid (Phosphoric_acid_II_3.96_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.505 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5549 (7) Å	Neutron radiation
b = 8.3362 (12) Å	T = 295 K
c = 14.1067 (18) Å	white
V = 535.64 (8) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.048	Weighting scheme based on measured s.u.'s
R(F^2) = 0.1104	(Δ/σ)max = 0.01
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.882 (3)	0.2885 (14)	−0.2306 (8)	0.0025 (10)*
O11	0.659 (4)	0.1592 (19)	−0.1991 (12)	0.0025 (10)*
D11	0.712 (6)	0.085 (3)	−0.1505 (15)	0.031 (3)*
O12	1.072 (4)	0.339 (2)	−0.1478 (11)	0.0025 (10)*
O13	0.717 (4)	0.4371 (17)	−0.2698 (13)	0.0025 (10)*
D13	0.653 (5)	0.521 (3)	−0.2291 (16)	0.031 (3)*
O14	1.076 (4)	0.215 (2)	−0.3097 (10)	0.0025 (10)*
D14	1.136 (6)	0.284 (3)	−0.3609 (14)	0.031 (3)*
P22	0.560 (3)	0.5115 (13)	−0.0020 (9)	0.0025 (10)*
O21	0.795 (3)	0.6420 (17)	0.0166 (13)	0.0025 (10)*
D21	0.991 (4)	0.609 (3)	0.031 (2)	0.031 (3)*
O22	0.460 (4)	0.529 (2)	−0.1064 (10)	0.0025 (10)*
D22	0.286 (5)	0.470 (3)	−0.1212 (16)	0.031 (3)*
O23	0.704 (4)	0.3445 (15)	0.0111 (13)	0.0025 (10)*
D23	0.650 (5)	0.283 (3)	0.0674 (16)	0.031 (3)*
O24	0.297 (3)	0.5293 (18)	0.0642 (11)	0.0025 (10)*

Geometric parameters (Å, º)

P11—O11	1.55 (2)	P22—O21	1.549 (19)
P11—O12	1.51 (2)	P22—O22	1.549 (19)
P11—O13	1.55 (2)	P22—O23	1.550 (18)
P11—O14	1.55 (2)	P22—O24	1.53 (2)
O11—D11	0.95 (3)	O21—D21	0.96 (2)
O13—D13	0.95 (3)	O22—D22	0.96 (3)
O14—D14	0.96 (3)	O23—D23	0.98 (3)
O11—P11—O12	110.4 (11)	O21—P22—O22	107.4 (12)
O11—P11—O13	109.9 (12)	O21—P22—O23	108.6 (12)
O11—P11—O14	107.8 (11)	O21—P22—O24	111.8 (11)
O12—P11—O13	109.3 (11)	O22—P22—O23	108.8 (12)
O12—P11—O14	109.9 (12)	O22—P22—O24	110.0 (12)
O13—P11—O14	109.6 (11)	O23—P22—O24	110.3 (11)
P11—O11—D11	120 (2)	P22—O21—D21	119 (2)
P11—O13—D13	121 (2)	P22—O22—D22	113.8 (19)
P11—O14—D14	118 (2)	P22—O23—D23	118 (2)
O12—P11—O11—D11	−32 (3)	O22—P22—O21—D21	−116 (3)
O13—P11—O11—D11	−153 (2)	O23—P22—O21—D21	2 (3)
O14—P11—O11—D11	88 (2)	O24—P22—O21—D21	124 (3)
O11—P11—O13—D13	87 (3)	O21—P22—O22—D22	−167 (2)
O12—P11—O13—D13	−34 (3)	O23—P22—O22—D22	76 (2)
O14—P11—O13—D13	−155 (2)	O24—P22—O22—D22	−45 (2)
O11—P11—O14—D14	143 (2)	O21—P22—O23—D23	108 (2)
O12—P11—O14—D14	−96 (2)	O22—P22—O23—D23	−136 (2)
O13—P11—O14—D14	24 (3)	O24—P22—O23—D23	−15 (3)

Phosphoric acid (Phosphoric_acid_II_4.36_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.526 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5456 (7) Å	Neutron radiation
b = 8.3104 (13) Å	T = 295 K
c = 14.0631 (19) Å	white
V = 531.25 (8) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.046	Weighting scheme based on measured s.u.'s
R(F^2) = 0.106	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.883 (3)	0.2869 (15)	−0.2313 (8)	0.0027 (10)*
O11	0.658 (4)	0.160 (2)	−0.1975 (13)	0.0027 (10)*
D11	0.701 (7)	0.080 (3)	−0.1505 (16)	0.034 (3)*
O12	1.074 (4)	0.340 (2)	−0.1490 (11)	0.0027 (10)*
O13	0.720 (4)	0.4341 (18)	−0.2737 (13)	0.0027 (10)*
D13	0.659 (5)	0.517 (3)	−0.2313 (17)	0.034 (3)*
O14	1.074 (4)	0.208 (2)	−0.3098 (11)	0.0027 (10)*
D14	1.136 (7)	0.286 (3)	−0.3566 (16)	0.034 (3)*
P22	0.566 (3)	0.5124 (13)	−0.0019 (9)	0.0027 (10)*
O21	0.798 (4)	0.6451 (17)	0.0158 (14)	0.0027 (10)*
D21	0.990 (4)	0.608 (3)	0.036 (2)	0.034 (3)*
O22	0.464 (4)	0.528 (2)	−0.1068 (10)	0.0027 (10)*
D22	0.293 (5)	0.464 (4)	−0.1196 (17)	0.034 (3)*
O23	0.716 (4)	0.3470 (16)	0.0140 (14)	0.0027 (10)*
D23	0.640 (5)	0.284 (3)	0.0666 (17)	0.034 (3)*
O24	0.300 (3)	0.5287 (19)	0.0637 (11)	0.0027 (10)*

Geometric parameters (Å, º)

P11—O11	1.54 (2)	P22—O21	1.55 (2)
P11—O12	1.51 (2)	P22—O22	1.552 (19)
P11—O13	1.55 (2)	P22—O23	1.551 (19)
P11—O14	1.55 (2)	P22—O24	1.53 (2)
O11—D11	0.96 (3)	O21—D21	0.97 (3)
O13—D13	0.95 (3)	O22—D22	0.96 (3)
O14—D14	0.97 (3)	O23—D23	0.97 (3)
O11—P11—O12	110.1 (12)	O21—P22—O22	107.3 (12)
O11—P11—O13	109.9 (12)	O21—P22—O23	108.0 (12)
O11—P11—O14	107.5 (12)	O21—P22—O24	112.3 (12)
O12—P11—O13	109.8 (12)	O22—P22—O23	110.0 (12)
O12—P11—O14	110.3 (12)	O22—P22—O24	109.3 (12)
O13—P11—O14	109.1 (11)	O23—P22—O24	109.9 (12)
P11—O11—D11	124 (2)	P22—O21—D21	115.8 (19)
P11—O13—D13	118 (2)	P22—O22—D22	112 (2)
P11—O14—D14	111 (2)	P22—O23—D23	116 (2)
O12—P11—O11—D11	−36 (3)	O22—P22—O21—D21	−121 (3)
O13—P11—O11—D11	−157 (2)	O23—P22—O21—D21	−3 (3)
O14—P11—O11—D11	84 (3)	O24—P22—O21—D21	119 (2)
O11—P11—O13—D13	86 (2)	O21—P22—O22—D22	−169 (2)
O12—P11—O13—D13	−35 (3)	O23—P22—O22—D22	74 (3)
O14—P11—O13—D13	−156 (2)	O24—P22—O22—D22	−47 (3)
O11—P11—O14—D14	148 (2)	O21—P22—O23—D23	116 (2)
O12—P11—O14—D14	−92 (2)	O22—P22—O23—D23	−128 (2)
O13—P11—O14—D14	29 (3)	O24—P22—O23—D23	−7 (3)

Phosphoric acid (Phosphoric_acid_II_5.02_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.558 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5338 (7) Å	Neutron radiation
b = 8.2726 (12) Å	T = 295 K
c = 13.9867 (18) Å	white
V = 524.58 (8) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.039	Weighting scheme based on measured s.u.'s
R(F^2) = 0.0868	(Δ/σ)max = 0.04
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.880 (3)	0.2867 (14)	−0.2328 (8)	0.0015 (9)*
O11	0.655 (3)	0.1579 (19)	−0.1992 (11)	0.0015 (9)*
D11	0.702 (6)	0.090 (3)	−0.1476 (15)	0.035 (3)*
O12	1.069 (4)	0.338 (2)	−0.1492 (11)	0.0015 (9)*
O13	0.717 (4)	0.4371 (17)	−0.2730 (13)	0.0015 (9)*
D13	0.649 (5)	0.518 (3)	−0.2313 (17)	0.035 (3)*
O14	1.068 (4)	0.209 (2)	−0.3127 (11)	0.0015 (9)*
D14	1.134 (6)	0.289 (3)	−0.3583 (15)	0.035 (3)*
P22	0.568 (3)	0.5128 (13)	−0.0009 (9)	0.0015 (9)*
O21	0.804 (4)	0.6450 (17)	0.0146 (13)	0.0015 (9)*
D21	1.001 (4)	0.612 (3)	0.0331 (18)	0.035 (3)*
O22	0.462 (3)	0.533 (2)	−0.1055 (9)	0.0015 (9)*
D22	0.289 (5)	0.471 (3)	−0.1207 (16)	0.035 (3)*
O23	0.717 (4)	0.3453 (15)	0.0116 (13)	0.0015 (9)*
D23	0.651 (5)	0.281 (3)	0.0668 (16)	0.035 (3)*
O24	0.303 (3)	0.5285 (18)	0.0664 (10)	0.0015 (9)*

Geometric parameters (Å, º)

P11—O11	1.548 (19)	P22—O21	1.55 (2)
P11—O12	1.51 (2)	P22—O22	1.549 (18)
P11—O13	1.55 (2)	P22—O23	1.551 (18)
P11—O14	1.55 (2)	P22—O24	1.532 (19)
O11—D11	0.94 (3)	O21—D21	0.97 (3)
O13—D13	0.94 (3)	O22—D22	0.96 (3)
O14—D14	0.97 (3)	O23—D23	0.98 (3)
O11—P11—O12	109.4 (11)	O21—P22—O22	105.7 (11)
O11—P11—O13	110.4 (12)	O21—P22—O23	108.4 (12)
O11—P11—O14	107.3 (11)	O21—P22—O24	113.4 (11)
O12—P11—O13	109.0 (11)	O22—P22—O23	109.8 (11)
O12—P11—O14	111.3 (12)	O22—P22—O24	109.1 (11)
O13—P11—O14	109.5 (11)	O23—P22—O24	110.4 (11)
P11—O11—D11	120 (2)	P22—O21—D21	118.4 (19)
P11—O13—D13	120 (2)	P22—O22—D22	113.9 (18)
P11—O14—D14	111 (2)	P22—O23—D23	116 (2)
O12—P11—O11—D11	−29 (3)	O22—P22—O21—D21	−121 (2)
O13—P11—O11—D11	−148 (2)	O23—P22—O21—D21	−4 (3)
O14—P11—O11—D11	92 (2)	O24—P22—O21—D21	119 (2)
O11—P11—O13—D13	84 (2)	O21—P22—O22—D22	−169 (2)
O12—P11—O13—D13	−37 (3)	O23—P22—O22—D22	74 (2)
O14—P11—O13—D13	−159 (2)	O24—P22—O22—D22	−47 (2)
O11—P11—O14—D14	150 (2)	O21—P22—O23—D23	114 (2)
O12—P11—O14—D14	−91 (2)	O22—P22—O23—D23	−131 (2)
O13—P11—O14—D14	30 (2)	O24—P22—O23—D23	−11 (2)

Phosphoric acid (Phosphoric_acid_II_5.66_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.59 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5214 (6) Å	Neutron radiation
b = 8.2332 (11) Å	T = 295 K
c = 13.9189 (16) Å	white
V = 518.14 (7) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.041	Weighting scheme based on measured s.u.'s
R(F^2) = 0.0562	(Δ/σ)max = 0.04
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.876 (2)	0.2867 (13)	−0.2339 (7)	0.0013 (8)*
O11	0.652 (3)	0.1565 (17)	−0.2001 (10)	0.0013 (8)*
D11	0.719 (5)	0.088 (2)	−0.1497 (13)	0.0183 (17)*
O12	1.063 (3)	0.3366 (18)	−0.1490 (9)	0.0013 (8)*
O13	0.717 (3)	0.4374 (15)	−0.2767 (11)	0.0013 (8)*
D13	0.651 (3)	0.519 (2)	−0.2371 (13)	0.0183 (17)*
O14	1.068 (3)	0.2041 (19)	−0.3120 (9)	0.0013 (8)*
D14	1.137 (5)	0.285 (2)	−0.3579 (11)	0.0183 (17)*
P22	0.568 (2)	0.5171 (11)	−0.0003 (7)	0.0013 (8)*
O21	0.804 (3)	0.6502 (15)	0.0173 (11)	0.0013 (8)*
D21	1.003 (3)	0.616 (2)	0.0323 (14)	0.0183 (17)*
O22	0.464 (3)	0.5359 (18)	−0.1059 (8)	0.0013 (8)*
D22	0.294 (4)	0.470 (3)	−0.1217 (12)	0.0183 (17)*
O23	0.713 (3)	0.3474 (13)	0.0122 (11)	0.0013 (8)*
D23	0.641 (4)	0.281 (2)	0.0653 (13)	0.0183 (17)*
O24	0.304 (3)	0.5330 (16)	0.0655 (9)	0.0013 (8)*

Geometric parameters (Å, º)

P11—O11	1.548 (17)	P22—O21	1.549 (16)
P11—O12	1.510 (16)	P22—O22	1.551 (15)
P11—O13	1.553 (17)	P22—O23	1.553 (15)
P11—O14	1.549 (17)	P22—O24	1.510 (16)
O11—D11	0.95 (2)	O21—D21	0.97 (2)
O13—D13	0.92 (2)	O22—D22	0.97 (2)
O14—D14	0.97 (2)	O23—D23	0.98 (2)
O11—P11—O12	108.5 (9)	O21—P22—O22	106.8 (9)
O11—P11—O13	111.5 (9)	O21—P22—O23	109.1 (9)
O11—P11—O14	106.0 (10)	O21—P22—O24	112.8 (9)
O12—P11—O13	110.0 (10)	O22—P22—O23	108.9 (10)
O12—P11—O14	110.8 (9)	O22—P22—O24	109.1 (9)
O13—P11—O14	110.0 (10)	O23—P22—O24	110.1 (9)
P11—O11—D11	115.3 (17)	P22—O21—D21	118.0 (15)
P11—O13—D13	120.3 (17)	P22—O22—D22	113.6 (15)
P11—O14—D14	109.9 (17)	P22—O23—D23	116.6 (16)
O12—P11—O11—D11	−32 (2)	O22—P22—O21—D21	−116.8 (19)
O13—P11—O11—D11	−152.9 (17)	O23—P22—O21—D21	1 (2)
O14—P11—O11—D11	87.4 (18)	O24—P22—O21—D21	123.5 (19)
O11—P11—O13—D13	84.7 (18)	O21—P22—O22—D22	−170.7 (16)
O12—P11—O13—D13	−35.7 (19)	O23—P22—O22—D22	71.6 (18)
O14—P11—O13—D13	−158.0 (16)	O24—P22—O22—D22	−48.6 (19)
O11—P11—O14—D14	150.7 (17)	O21—P22—O23—D23	115.2 (18)
O12—P11—O14—D14	−91.8 (18)	O22—P22—O23—D23	−128.6 (17)
O13—P11—O14—D14	30.0 (19)	O24—P22—O23—D23	−9 (2)

Phosphoric acid (Phosphoric_acid_II_6.26_GPa)

Crystal data

D3O4P	Z = 8
Mr = 101.01	Cell parameters included in refinement
Orthorhombic, P212121	Dx = 2.617 Mg m^−3
Hall symbol: P 2ac 2ab	Melting point: 315.5 K K
a = 4.5121 (7) Å	Neutron radiation
b = 8.2009 (12) Å	T = 295 K
c = 13.8569 (17) Å	white
V = 512.75 (7) Å^3

Data collection

PEARL diffractometer	Data collection mode: transmission
Radiation source: Pulsed neutron source	Scan method: Time-of-flight
None monochromator	Absorption correction: empirical (using intensity measurements) Calculated using custom ISIS routines.
Specimen mounting: TiZr Capsule

Refinement

Least-squares matrix: full	55 restraints
Rwp = 0.111	Weighting scheme based on measured s.u.'s
R(F^2) = 0.0511	(Δ/σ)max = 0.02
Profile function: Voigt function convoluted with a back-to-back double exponential.	Background function: Chebychev polynomial
84 parameters	Preferred orientation correction: No requirement for preferred orientation correction

Special details

Refinement. Geometric restraints are detailed in the manuscript.

———————————————————————————— Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed Please Check

RESPONSE: The time of flight method was used

PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note

RESPONSE: No action taken.

————————————————————————————

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

	x	y	z	Uiso*/Ueq
P11	0.879 (3)	0.2851 (13)	−0.2328 (7)	0.0016 (9)*
O11	0.655 (3)	0.1522 (17)	−0.2017 (9)	0.0016 (9)*
D11	0.708 (5)	0.098 (2)	−0.1439 (12)	0.0206 (19)*
O12	1.065 (3)	0.3318 (18)	−0.1470 (9)	0.0016 (9)*
O13	0.718 (4)	0.4394 (15)	−0.2706 (11)	0.0016 (9)*
D13	0.649 (4)	0.533 (2)	−0.2407 (13)	0.0206 (19)*
O14	1.069 (3)	0.211 (2)	−0.3147 (9)	0.0016 (9)*
D14	1.139 (5)	0.291 (2)	−0.3597 (12)	0.0206 (19)*
P22	0.570 (2)	0.5197 (11)	0.0000 (7)	0.0016 (9)*
O21	0.799 (3)	0.6564 (15)	0.0194 (12)	0.0016 (9)*
D21	1.001 (4)	0.620 (2)	0.0275 (15)	0.0206 (19)*
O22	0.464 (3)	0.5356 (18)	−0.1060 (8)	0.0016 (9)*
D22	0.290 (4)	0.477 (3)	−0.1255 (12)	0.0206 (19)*
O23	0.719 (3)	0.3511 (14)	0.0153 (12)	0.0016 (9)*
D23	0.649 (4)	0.277 (2)	0.0650 (13)	0.0206 (19)*
O24	0.305 (3)	0.5345 (16)	0.0639 (9)	0.0016 (9)*

Geometric parameters (Å, º)

P11—O11	1.548 (17)	P22—O21	1.548 (16)
P11—O12	1.505 (16)	P22—O22	1.550 (15)
P11—O13	1.550 (17)	P22—O23	1.552 (15)
P11—O14	1.547 (17)	P22—O24	1.493 (16)
O11—D11	0.95 (2)	O21—D21	0.97 (2)
O13—D13	0.93 (2)	O22—D22	0.96 (2)
O14—D14	0.96 (2)	O23—D23	0.97 (2)
O11—P11—O12	108.9 (9)	O21—P22—O22	108.0 (10)
O11—P11—O13	111.3 (10)	O21—P22—O23	109.4 (9)
O11—P11—O14	106.8 (10)	O21—P22—O24	111.9 (9)
O12—P11—O13	108.7 (10)	O22—P22—O23	109.8 (10)
O12—P11—O14	111.8 (9)	O22—P22—O24	107.9 (9)
O13—P11—O14	109.4 (10)	O23—P22—O24	109.8 (9)
P11—O11—D11	113.7 (17)	P22—O21—D21	115.2 (15)
P11—O13—D13	133.1 (18)	P22—O22—D22	118.5 (15)
P11—O14—D14	113.0 (17)	P22—O23—D23	120.9 (16)
O12—P11—O11—D11	−19 (2)	O22—P22—O21—D21	−110 (2)
O13—P11—O11—D11	−138.8 (17)	O23—P22—O21—D21	9 (2)
O14—P11—O11—D11	101.9 (18)	O24—P22—O21—D21	131.2 (19)
O11—P11—O13—D13	89 (3)	O21—P22—O22—D22	−166 (2)
O12—P11—O13—D13	−31 (3)	O23—P22—O22—D22	75 (2)
O14—P11—O13—D13	−153 (2)	O24—P22—O22—D22	−45 (2)
O11—P11—O14—D14	150.3 (18)	O21—P22—O23—D23	117.7 (19)
O12—P11—O14—D14	−90.7 (19)	O22—P22—O23—D23	−123.9 (19)
O13—P11—O14—D14	30 (2)	O24—P22—O23—D23	−5 (2)