Phase behaviour and thermoelastic properties of perdeuterated ammonia hydrate and ice polymorphs from 0 to 2 GPa

Fortes, A.D.; Wood, I.G.; Vočadlo, L.; Knight, K.S.; Marshall, W.G.; Tucker, M.G.; Fernandez-Alonso, F.

doi:10.1107/S0021889809027897

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Phase behaviour and thermoelastic properties of perdeuterated ammonia hydrate and ice polymorphs from 0 to 2 GPa

A. D. Fortes, I. G. Wood, L. Vočadlo, K. S. Knight, W. G. Marshall, M. G. Tucker and F. Fernandez-Alonso

The results are described of a series of neutron powder diffraction experiments over the pressure and temperature ranges 0 < P < 2 GPa, 150 < T < 240 K, which were carried out with the objective of determining the phase behaviour and thermoelastic properties of perdeuterated ammonia dihydrate (ND₃·2D₂O). In addition to the low-pressure cubic crystalline phase, ADH I, two closely related monoclinic polymorphs of ammonia dihydrate have been identified, which commonly occur as a composite in the range 450–550 MPa at 175 K; these are labelled ADH IIa and IIb, and each has unit-cell volume V ≃ 310 Å³ and number of formula units per unit cell Z = 4. It has been determined that this composite dissociates to a mixture of ammonia monohydrate (ND₃·D₂O) phase II (AMH II) and ice II when warmed to ∼190 K at 550 MPa, which in turn partially melts to ice II + liquid at T = 196 K; AMH II has a large orthorhombic unit cell (V ≃ 890 Å³, Z = 16). Above 600 MPa, an orthorhombic polymorph of ammonia dihydrate (with V ≃ 530 Å³, Z = 8), which has been referred to previously as ADH IV, persists to pressures greater than 2 GPa and appears to be the liquidus phase over this whole pressure range. This phase has been observed co-existing with ice II, ice VI and AMH II. The most plausible synthesis of the high-pressure phase behaviour is described here. This model explains the reported observations, and provides measurements of the densities, thermal expansion, bulk moduli and crystal growth kinetics of the high-pressure ammonia dihydrate, ammonia monohydrate and ice polymorphs.

Keywords: ammonia dihydrate; ammonia monohydrate; ice; neutron diffraction; polymorphism; crystal growth kinetics.

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Supporting information

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889809027897/ks5224sup1.cif
Contains datablocks G25904_913_AL_ICEIX_publ, 45470_81B_publ, G25904_913_AL_ICEIX_overall, G25904_913_AL_ICEIX_phase_1, G25904_913_AL_ICEIX_phase_2, G25904_913_AL_ICEIX_phase_3, G25904_913_AL_ICEIX_phase_4, G25904_913_AL_ICEIX_phase_5, 45470_81B_overall, 45470_81B_phase_3, 45470_81B_phase_4, 45470_81B_phase_6, G25904_913_AL_ICEIX_p_01, G25904_913_AL_ICEIX_p_02, 45470_81B_phase_1, 45470_81B_phase_2, 45470_81B_phase_5, 45470_81B_p_01

Portable Document Format (PDF) file https://doi.org/10.1107/S0021889809027897/ks5224sup2.pdf
Supplementary material

Computing details top

Figures top

(G25904_913_AL_ICEIX_phase_1) top

Crystal data top

D	β = 102.1043 (10)°
M_r = 2.01	V = 310.93 (1) Å³
Monoclinic, P2₁/n	Z = 2
a = 7.78366 (9) Å	? radiation, λ = ? Å
b = 6.72568 (7) Å	?; ?, ?; ? × ?; ? mm
c = 6.07443 (8) Å

Data collection top

Refinement top

Least-squares matrix: full	1684 data points
R_p = 0.021	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 1455.7 #6 (sig-2) = 20.8 #7 (gam-0) = 0.00 #8 (gam-1) = 42.61 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.208 #19(L12) = -0.203 #20(L13) = 0.050 #21(L23) = 0.163 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 3270.9 #6 (sig-2) = -140.1 #7 (gam-0) = 0.00 #8 (gam-1) = 25.89 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.190 #20(L13) = 0.257 #21(L23) = 0.237 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 386.5 #7 (gam-0) = 0.00 #8 (gam-1) = 9.43 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 10.0 #6 (sig-2) = 1082.3 #7 (gam-0) = 0.00 #8 (gam-1) = 126.68 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 14 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 296.3 #7 (gam-0) = 0.00 #8 (gam-1) = 6.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.019	14 parameters
R_exp = 0.012	0 restraints
R(F²) = 0.19600	(Δ/σ)_max = 0.04
χ² = 1.877	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 1.47034 2: -9.966650E-02 3: 0.333141 4: -1.291320E-02 5: 0.146189 6: -8.428790E-04 7: 4.640750E-02 8: 7.992300E-03 9: 8.360310E-0310: 3.222010E-0211: 1.685810E-0212: 3.469840E-02

Crystal data top

D	β = 102.1043 (10)°
M_r = 2.01	V = 310.93 (1) Å³
Monoclinic, P2₁/n	Z = 2
a = 7.78366 (9) Å	? radiation, λ = ? Å
b = 6.72568 (7) Å	?; ?, ?; ? × ?; ? mm
c = 6.07443 (8) Å

Data collection top

Refinement top

R_p = 0.021	χ² = 1.877
R_wp = 0.019	1684 data points
R_exp = 0.012	14 parameters
R(F²) = 0.19600	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
dummy	0.0	0.0	0.0	0.025*

(G25904_913_AL_ICEIX_phase_2) top

Crystal data top

D	c = 6.85885 (10) Å
M_r = 2.01	V = 899.12 (2) Å³
Orthorhombic, Pbca	Z = 4
a = 18.8679 (2) Å	? radiation, λ = ? Å
b = 6.94772 (9) Å	?; ?, ?; ? × ?; ? mm

Data collection top

Refinement top

Least-squares matrix: full	1684 data points
R_p = 0.021	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 1455.7 #6 (sig-2) = 20.8 #7 (gam-0) = 0.00 #8 (gam-1) = 42.61 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.208 #19(L12) = -0.203 #20(L13) = 0.050 #21(L23) = 0.163 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 3270.9 #6 (sig-2) = -140.1 #7 (gam-0) = 0.00 #8 (gam-1) = 25.89 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.190 #20(L13) = 0.257 #21(L23) = 0.237 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 386.5 #7 (gam-0) = 0.00 #8 (gam-1) = 9.43 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 10.0 #6 (sig-2) = 1082.3 #7 (gam-0) = 0.00 #8 (gam-1) = 126.68 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 14 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 296.3 #7 (gam-0) = 0.00 #8 (gam-1) = 6.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.019	14 parameters
R_exp = 0.012	0 restraints
R(F²) = 0.19600	(Δ/σ)_max = 0.04
χ² = 1.877	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 1.47034 2: -9.966650E-02 3: 0.333141 4: -1.291320E-02 5: 0.146189 6: -8.428790E-04 7: 4.640750E-02 8: 7.992300E-03 9: 8.360310E-0310: 3.222010E-0211: 1.685810E-0212: 3.469840E-02

Crystal data top

D	c = 6.85885 (10) Å
M_r = 2.01	V = 899.12 (2) Å³
Orthorhombic, Pbca	Z = 4
a = 18.8679 (2) Å	? radiation, λ = ? Å
b = 6.94772 (9) Å	?; ?, ?; ? × ?; ? mm

Data collection top

Refinement top

R_p = 0.021	χ² = 1.877
R_wp = 0.019	1684 data points
R_exp = 0.012	14 parameters
R(F²) = 0.19600	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
dummy	0.0	0.0	0.0	0.025*

(G25904_913_AL_ICEIX_phase_3) top

Crystal data top

D₂O	V = 886.99 (2) Å³
M_r = 20.03	Z = 36
Trigonal, R3	? radiation, λ = ? Å
a = 12.87078 (12) Å	?; ?, ?; ? × ?; ? mm
c = 6.1827 (1) Å

Data collection top

Refinement top

Least-squares matrix: full	1684 data points
R_p = 0.021	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 1455.7 #6 (sig-2) = 20.8 #7 (gam-0) = 0.00 #8 (gam-1) = 42.61 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.208 #19(L12) = -0.203 #20(L13) = 0.050 #21(L23) = 0.163 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 3270.9 #6 (sig-2) = -140.1 #7 (gam-0) = 0.00 #8 (gam-1) = 25.89 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.190 #20(L13) = 0.257 #21(L23) = 0.237 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 386.5 #7 (gam-0) = 0.00 #8 (gam-1) = 9.43 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 10.0 #6 (sig-2) = 1082.3 #7 (gam-0) = 0.00 #8 (gam-1) = 126.68 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 14 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 296.3 #7 (gam-0) = 0.00 #8 (gam-1) = 6.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.019	14 parameters
R_exp = 0.012	0 restraints
R(F²) = 0.19600	(Δ/σ)_max = 0.04
χ² = 1.877	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 1.47034 2: -9.966650E-02 3: 0.333141 4: -1.291320E-02 5: 0.146189 6: -8.428790E-04 7: 4.640750E-02 8: 7.992300E-03 9: 8.360310E-0310: 3.222010E-0211: 1.685810E-0212: 3.469840E-02

Crystal data top

D₂O	V = 886.99 (2) Å³
M_r = 20.03	Z = 36
Trigonal, R3	? radiation, λ = ? Å
a = 12.87078 (12) Å	?; ?, ?; ? × ?; ? mm
c = 6.1827 (1) Å

Data collection top

Refinement top

R_p = 0.021	χ² = 1.877
R_wp = 0.019	1684 data points
R_exp = 0.012	14 parameters
R(F²) = 0.19600	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
O1	0.21637	0.19055	0.02085	0.02*
O2	0.19533	0.23519	0.48044	0.02*
D1	0.14865	0.19305	−0.01953	0.02*
D2	0.22888	0.21722	0.19653	0.02*
D3	0.10598	0.21062	0.48697	0.02*
D4	0.24751	0.31406	0.54313	0.02*

(G25904_913_AL_ICEIX_phase_4) top

Crystal data top

Al	V = 65.79 (1) Å³
M_r = 26.98	Z = 4
Cubic, Fm3m	? radiation, λ = ? Å
a = 4.03702 (12) Å	?; ?, ?; ? × ?; ? mm

Data collection top

Refinement top

Least-squares matrix: full	1684 data points
R_p = 0.021	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 1455.7 #6 (sig-2) = 20.8 #7 (gam-0) = 0.00 #8 (gam-1) = 42.61 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.208 #19(L12) = -0.203 #20(L13) = 0.050 #21(L23) = 0.163 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 3270.9 #6 (sig-2) = -140.1 #7 (gam-0) = 0.00 #8 (gam-1) = 25.89 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.190 #20(L13) = 0.257 #21(L23) = 0.237 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 386.5 #7 (gam-0) = 0.00 #8 (gam-1) = 9.43 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 10.0 #6 (sig-2) = 1082.3 #7 (gam-0) = 0.00 #8 (gam-1) = 126.68 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 14 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 296.3 #7 (gam-0) = 0.00 #8 (gam-1) = 6.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.019	14 parameters
R_exp = 0.012	0 restraints
R(F²) = 0.19600	(Δ/σ)_max = 0.04
χ² = 1.877	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 1.47034 2: -9.966650E-02 3: 0.333141 4: -1.291320E-02 5: 0.146189 6: -8.428790E-04 7: 4.640750E-02 8: 7.992300E-03 9: 8.360310E-0310: 3.222010E-0211: 1.685810E-0212: 3.469840E-02

Crystal data top

Al	V = 65.79 (1) Å³
M_r = 26.98	Z = 4
Cubic, Fm3m	? radiation, λ = ? Å
a = 4.03702 (12) Å	?; ?, ?; ? × ?; ? mm

Data collection top

Refinement top

R_p = 0.021	χ² = 1.877
R_wp = 0.019	1684 data points
R_exp = 0.012	14 parameters
R(F²) = 0.19600	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Al	0.0	0.0	0.0	0.01*

(G25904_913_AL_ICEIX_phase_5) top

Crystal data top

D₂O	V = 297.79 (1) Å³
M_r = 20.03	Z = 12
Tetragonal, P4₁2₁2	? radiation, λ = ? Å
a = 6.6748 (3) Å	?; ?, ?; ? × ?; ? mm
c = 6.6838 (6) Å

Data collection top

Refinement top

Least-squares matrix: full	1684 data points
R_p = 0.021	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 1455.7 #6 (sig-2) = 20.8 #7 (gam-0) = 0.00 #8 (gam-1) = 42.61 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.208 #19(L12) = -0.203 #20(L13) = 0.050 #21(L23) = 0.163 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 3270.9 #6 (sig-2) = -140.1 #7 (gam-0) = 0.00 #8 (gam-1) = 25.89 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.190 #20(L13) = 0.257 #21(L23) = 0.237 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 386.5 #7 (gam-0) = 0.00 #8 (gam-1) = 9.43 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 10.0 #6 (sig-2) = 1082.3 #7 (gam-0) = 0.00 #8 (gam-1) = 126.68 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 14 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.1359 #2 (bet-0) = 0.021086 #3 (bet-1) = 0.011943 #4 (sig-0) = 0.0 #5 (sig-1) = 930.7 #6 (sig-2) = 296.3 #7 (gam-0) = 0.00 #8 (gam-1) = 6.81 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.019	14 parameters
R_exp = 0.012	0 restraints
R(F²) = 0.19600	(Δ/σ)_max = 0.04
χ² = 1.877	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 1.47034 2: -9.966650E-02 3: 0.333141 4: -1.291320E-02 5: 0.146189 6: -8.428790E-04 7: 4.640750E-02 8: 7.992300E-03 9: 8.360310E-0310: 3.222010E-0211: 1.685810E-0212: 3.469840E-02

Crystal data top

D₂O	V = 297.79 (1) Å³
M_r = 20.03	Z = 12
Tetragonal, P4₁2₁2	? radiation, λ = ? Å
a = 6.6748 (3) Å	?; ?, ?; ? × ?; ? mm
c = 6.6838 (6) Å

Data collection top

Refinement top

R_p = 0.021	χ² = 1.877
R_wp = 0.019	1684 data points
R_exp = 0.012	14 parameters
R(F²) = 0.19600	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
O1	0.113	0.311	0.287	0.062*
O2	0.397	0.397	0.0	0.044*
D1	−0.004	0.338	0.243	0.072*
D2	0.109	0.182	0.318	0.068*
D3	0.29	0.358	0.102	0.047*

(45470_81B_phase_1) top

Crystal data top

D_10.00O₅	V = 218.72 (5) Å³
M_r = 100.13	Z = 2
Tetragonal, P4₂/nmc	? radiation, λ = ? Å
a = 6.1860 (8) Å	?, ? × ? × ? mm
c = 5.7157 (16) Å

Data collection top

Refinement top

Least-squares matrix: full	2528 data points
R_p = 0.034	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 80.0 #6 (sig-2) = 1.4 #7 (gam-0) = 0.00 #8 (gam-1) = 7.20 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026590 #3 (bet-1) = 0.026480 #4 (sig-0) = 0.0 #5 (sig-1) = 76.4 #6 (sig-2) = 1.5 #7 (gam-0) = 0.00 #8 (gam-1) = 2.73 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 139.4 #6 (sig-2) = -9.1 #7 (gam-0) = 0.00 #8 (gam-1) = 13.63 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.024	8 parameters
R_exp = 0.016	0 restraints
R(F²) = 0.53681	(Δ/σ)_max = 0.08
χ² = 2.372	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 0.675803 2: 0.147386 3: 0.233697 4: 8.198550E-03 5: 2.032030E-02 6: 1.054060E-03 7: -7.461600E-03 8: -1.286660E-02 9: -2.389770E-0210: -2.848430E-0311: -1.792420E-0212: 2.407580E-03

Crystal data top

D_10.00O₅	V = 218.72 (5) Å³
M_r = 100.13	Z = 2
Tetragonal, P4₂/nmc	? radiation, λ = ? Å
a = 6.1860 (8) Å	?, ? × ? × ? mm
c = 5.7157 (16) Å

Data collection top

Refinement top

R_p = 0.034	χ² = 2.372
R_wp = 0.024	2528 data points
R_exp = 0.016	8 parameters
R(F²) = 0.53681	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
O1	0.75	0.25	0.75	0.025*
O2	0.75	0.5295	0.1339	0.025*
D1	0.75	0.4628	−0.0137	0.025*	0.5
D2	0.75	0.3703	−0.1365	0.025*	0.5
D3	0.75	0.6872	0.1248	0.025*	0.5
D4	0.1325	0.5307	0.7844	0.025*	0.5

(45470_81B_phase_2) top

Crystal data top

Pb	V = 118.43 (1) Å³
M_r = 203.97	Z = 4
Cubic, Fm3m	? radiation, λ = ? Å
a = 4.9108 (2) Å	?, ? × ? × ? mm

Data collection top

Refinement top

Least-squares matrix: full	2528 data points
R_p = 0.034	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 80.0 #6 (sig-2) = 1.4 #7 (gam-0) = 0.00 #8 (gam-1) = 7.20 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026590 #3 (bet-1) = 0.026480 #4 (sig-0) = 0.0 #5 (sig-1) = 76.4 #6 (sig-2) = 1.5 #7 (gam-0) = 0.00 #8 (gam-1) = 2.73 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 139.4 #6 (sig-2) = -9.1 #7 (gam-0) = 0.00 #8 (gam-1) = 13.63 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.024	8 parameters
R_exp = 0.016	0 restraints
R(F²) = 0.53681	(Δ/σ)_max = 0.08
χ² = 2.372	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 0.675803 2: 0.147386 3: 0.233697 4: 8.198550E-03 5: 2.032030E-02 6: 1.054060E-03 7: -7.461600E-03 8: -1.286660E-02 9: -2.389770E-0210: -2.848430E-0311: -1.792420E-0212: 2.407580E-03

Crystal data top

Pb	V = 118.43 (1) Å³
M_r = 203.97	Z = 4
Cubic, Fm3m	? radiation, λ = ? Å
a = 4.9108 (2) Å	?, ? × ? × ? mm

Data collection top

Refinement top

R_p = 0.034	χ² = 2.372
R_wp = 0.024	2528 data points
R_exp = 0.016	8 parameters
R(F²) = 0.53681	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pb	0.0	0.0	0.0	0.025*

(45470_81B_phase_3) top

Crystal data top

CW	V = 20.70 (1) Å³
M_r = 195.86	Z = 1
Hexagonal, P6m2	? radiation, λ = ? Å
a = 2.9016 (3) Å	?, ? × ? × ? mm
c = 2.83867 (12) Å

Data collection top

Refinement top

Least-squares matrix: full	2528 data points
R_p = 0.034	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 80.0 #6 (sig-2) = 1.4 #7 (gam-0) = 0.00 #8 (gam-1) = 7.20 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026590 #3 (bet-1) = 0.026480 #4 (sig-0) = 0.0 #5 (sig-1) = 76.4 #6 (sig-2) = 1.5 #7 (gam-0) = 0.00 #8 (gam-1) = 2.73 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 139.4 #6 (sig-2) = -9.1 #7 (gam-0) = 0.00 #8 (gam-1) = 13.63 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.024	8 parameters
R_exp = 0.016	0 restraints
R(F²) = 0.53681	(Δ/σ)_max = 0.08
χ² = 2.372	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 0.675803 2: 0.147386 3: 0.233697 4: 8.198550E-03 5: 2.032030E-02 6: 1.054060E-03 7: -7.461600E-03 8: -1.286660E-02 9: -2.389770E-0210: -2.848430E-0311: -1.792420E-0212: 2.407580E-03

Crystal data top

CW	V = 20.70 (1) Å³
M_r = 195.86	Z = 1
Hexagonal, P6m2	? radiation, λ = ? Å
a = 2.9016 (3) Å	?, ? × ? × ? mm
c = 2.83867 (12) Å

Data collection top

Refinement top

R_p = 0.034	χ² = 2.372
R_wp = 0.024	2528 data points
R_exp = 0.016	8 parameters
R(F²) = 0.53681	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
C	0.66667	0.33333	0.5	0.025*
W	0.0	0.0	0.0	0.025*

(45470_81B_phase_4) top

Crystal data top

D	c = 6.3788 (3) Å
M_r = 2.01	V = 533.00 (4) Å³
Orthorhombic, Pncn	Z = 4
a = 12.5626 (11) Å	? radiation, λ = ? Å
b = 6.6513 (3) Å	?, ? × ? × ? mm

Data collection top

Refinement top

Least-squares matrix: full	2528 data points
R_p = 0.034	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 80.0 #6 (sig-2) = 1.4 #7 (gam-0) = 0.00 #8 (gam-1) = 7.20 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026590 #3 (bet-1) = 0.026480 #4 (sig-0) = 0.0 #5 (sig-1) = 76.4 #6 (sig-2) = 1.5 #7 (gam-0) = 0.00 #8 (gam-1) = 2.73 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 139.4 #6 (sig-2) = -9.1 #7 (gam-0) = 0.00 #8 (gam-1) = 13.63 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.024	8 parameters
R_exp = 0.016	0 restraints
R(F²) = 0.53681	(Δ/σ)_max = 0.08
χ² = 2.372	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 0.675803 2: 0.147386 3: 0.233697 4: 8.198550E-03 5: 2.032030E-02 6: 1.054060E-03 7: -7.461600E-03 8: -1.286660E-02 9: -2.389770E-0210: -2.848430E-0311: -1.792420E-0212: 2.407580E-03

Crystal data top

D	c = 6.3788 (3) Å
M_r = 2.01	V = 533.00 (4) Å³
Orthorhombic, Pncn	Z = 4
a = 12.5626 (11) Å	? radiation, λ = ? Å
b = 6.6513 (3) Å	?, ? × ? × ? mm

Data collection top

Refinement top

R_p = 0.034	χ² = 2.372
R_wp = 0.024	2528 data points
R_exp = 0.016	8 parameters
R(F²) = 0.53681	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
dummy	0.0	0.0	0.0	0.025*

(45470_81B_phase_5) top

Crystal data top

D	V = 265.69 Å³
M_r = 2.01	Z = 8
Tetragonal, I4₂d	? radiation, λ = ? Å
a = 8.15 Å	?, ? × ? × ? mm
c = 4.0 Å

Data collection top

Refinement top

Least-squares matrix: full	2528 data points
R_p = 0.034	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 80.0 #6 (sig-2) = 1.4 #7 (gam-0) = 0.00 #8 (gam-1) = 7.20 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026590 #3 (bet-1) = 0.026480 #4 (sig-0) = 0.0 #5 (sig-1) = 76.4 #6 (sig-2) = 1.5 #7 (gam-0) = 0.00 #8 (gam-1) = 2.73 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 139.4 #6 (sig-2) = -9.1 #7 (gam-0) = 0.00 #8 (gam-1) = 13.63 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.024	8 parameters
R_exp = 0.016	0 restraints
R(F²) = 0.53681	(Δ/σ)_max = 0.08
χ² = 2.372	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 0.675803 2: 0.147386 3: 0.233697 4: 8.198550E-03 5: 2.032030E-02 6: 1.054060E-03 7: -7.461600E-03 8: -1.286660E-02 9: -2.389770E-0210: -2.848430E-0311: -1.792420E-0212: 2.407580E-03

Crystal data top

D	V = 265.69 Å³
M_r = 2.01	Z = 8
Tetragonal, I4₂d	? radiation, λ = ? Å
a = 8.15 Å	?, ? × ? × ? mm
c = 4.0 Å

Data collection top

Refinement top

R_p = 0.034	χ² = 2.372
R_wp = 0.024	2528 data points
R_exp = 0.016	8 parameters
R(F²) = 0.53681	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
dummy	0.0	0.0	0.0	0.025*

(45470_81B_phase_6) top

Crystal data top

D₂O	V = 879.85 (13) Å³
M_r = 20.03	Z = 36
Trigonal, R3	? radiation, λ = ? Å
a = 12.8396 (10) Å	?, ? × ? × ? mm
c = 6.1628 (7) Å

Data collection top

Refinement top

Least-squares matrix: full	2528 data points
R_p = 0.034	Profile function: TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 80.0 #6 (sig-2) = 1.4 #7 (gam-0) = 0.00 #8 (gam-1) = 7.20 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026590 #3 (bet-1) = 0.026480 #4 (sig-0) = 0.0 #5 (sig-1) = 76.4 #6 (sig-2) = 1.5 #7 (gam-0) = 0.00 #8 (gam-1) = 2.73 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0, TOF Profile function number 3 with 21 terms Profile coefficients for exponential pseudovoigt convolution Von Dreele, 1990 (unpublished) #1 (alp ) = 0.2393 #2 (bet-0) = 0.026588 #3 (bet-1) = 0.026479 #4 (sig-0) = 0.0 #5 (sig-1) = 139.4 #6 (sig-2) = -9.1 #7 (gam-0) = 0.00 #8 (gam-1) = 13.63 #9 (gam-2) = 0.00 #10(gsf ) = 0.00 #11(g1ec ) = 0.00 #12(g2ec ) = 0.00 #13(rstr ) = 0.000 #14(rsta ) = 0.000 #15(rsca ) = 0.000 #16(L11) = 0.000 #17(L22) = 0.000 #18(L33) = 0.000 #19(L12) = 0.000 #20(L13) = 0.000 #21(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.024	8 parameters
R_exp = 0.016	0 restraints
R(F²) = 0.53681	(Δ/σ)_max = 0.08
χ² = 2.372	Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 0.675803 2: 0.147386 3: 0.233697 4: 8.198550E-03 5: 2.032030E-02 6: 1.054060E-03 7: -7.461600E-03 8: -1.286660E-02 9: -2.389770E-0210: -2.848430E-0311: -1.792420E-0212: 2.407580E-03

Crystal data top

D₂O	V = 879.85 (13) Å³
M_r = 20.03	Z = 36
Trigonal, R3	? radiation, λ = ? Å
a = 12.8396 (10) Å	?, ? × ? × ? mm
c = 6.1628 (7) Å

Data collection top

Refinement top

R_p = 0.034	χ² = 2.372
R_wp = 0.024	2528 data points
R_exp = 0.016	8 parameters
R(F²) = 0.53681	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
O1	0.21637	0.19055	0.02085	0.02*
O2	0.19533	0.23519	0.48044	0.02*
D1	0.14865	0.19305	−0.01953	0.02*
D2	0.22888	0.21722	0.19653	0.02*
D3	0.10598	0.21062	0.48697	0.02*
D4	0.24751	0.31406	0.54313	0.02*

Experimental details

	(G25904_913_AL_ICEIX_phase_1)	(G25904_913_AL_ICEIX_phase_2)	(G25904_913_AL_ICEIX_phase_3)	(G25904_913_AL_ICEIX_phase_4)
Crystal data
Chemical formula	D	D	D₂O	Al
M_r	2.01	2.01	20.03	26.98
Crystal system, space group	Monoclinic, P2₁/n	Orthorhombic, Pbca	Trigonal, R3	Cubic, Fm3m
Temperature (K)	?	?	?	?
a, b, c (Å)	7.78366 (9), 6.72568 (7), 6.07443 (8)	18.8679 (2), 6.94772 (9), 6.85885 (10)	12.87078 (12), 12.87078, 6.1827 (1)	4.03702 (12), 4.03702, 4.03702
α, β, γ (°)	90, 102.1043 (10), 90	90, 90, 90	90, 90, 120	90, 90, 90
V (Å³)	310.93 (1)	899.12 (2)	886.99 (2)	65.79 (1)
Z	2	4	36	4
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
Specimen shape, size (mm)	?; ?, ?; ? × ?; ?	?; ?, ?; ? × ?; ?	?; ?, ?; ? × ?; ?	?; ?, ?; ? × ?; ?

Data collection
Diffractometer	?; ?	?; ?	?; ?	?; ?
Specimen mounting	?; ?	?; ?	?; ?	?; ?
Data collection mode	?; ?	?; ?	?; ?	?; ?
Scan method	?; ?	?; ?	?; ?	?; ?
2θ values (°)	2θ_min = ? 2θ_max = ? 2θ_step = ?	2θ_min = ? 2θ_max = ? 2θ_step = ?	2θ_min = ? 2θ_max = ? 2θ_step = ?	2θ_min = ? 2θ_max = ? 2θ_step = ?

Refinement
R factors and goodness of fit	R_p = 0.021, R_wp = 0.019, R_exp = 0.012, R(F²) = 0.19600, χ² = 1.877	R_p = 0.021, R_wp = 0.019, R_exp = 0.012, R(F²) = 0.19600, χ² = 1.877	R_p = 0.021, R_wp = 0.019, R_exp = 0.012, R(F²) = 0.19600, χ² = 1.877	R_p = 0.021, R_wp = 0.019, R_exp = 0.012, R(F²) = 0.19600, χ² = 1.877
No. of data points	1684	1684	1684	1684
No. of parameters	14	14	14	14

	(G25904_913_AL_ICEIX_phase_5)	(45470_81B_phase_1)	(45470_81B_phase_2)	(45470_81B_phase_3)
Crystal data
Chemical formula	D₂O	D_10.00O₅	Pb	CW
M_r	20.03	100.13	203.97	195.86
Crystal system, space group	Tetragonal, P4₁2₁2	Tetragonal, P4₂/nmc	Cubic, Fm3m	Hexagonal, P6m2
Temperature (K)	?	?	?	?
a, b, c (Å)	6.6748 (3), 6.67484, 6.6838 (6)	6.1860 (8), 6.186, 5.7157 (16)	4.9108 (2), 4.91075, 4.91075	2.9016 (3), 2.90156, 2.83867 (12)
α, β, γ (°)	90, 90, 90	90, 90, 90	90, 90, 90	90, 90, 120
V (Å³)	297.79 (1)	218.72 (5)	118.43 (1)	20.70 (1)
Z	12	2	4	1
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
Specimen shape, size (mm)	?; ?, ?; ? × ?; ?	?, ? × ? × ?	?, ? × ? × ?	?, ? × ? × ?

Data collection
Diffractometer	?; ?	?	?	?
Specimen mounting	?; ?	?	?	?
Data collection mode	?; ?	?	?	?
Scan method	?; ?	?	?	?
2θ values (°)	2θ_min = ? 2θ_max = ? 2θ_step = ?	2θ_min = ? 2θ_max = ? 2θ_step = ?	2θ_min = ? 2θ_max = ? 2θ_step = ?	2θ_min = ? 2θ_max = ? 2θ_step = ?

Refinement
R factors and goodness of fit	R_p = 0.021, R_wp = 0.019, R_exp = 0.012, R(F²) = 0.19600, χ² = 1.877	R_p = 0.034, R_wp = 0.024, R_exp = 0.016, R(F²) = 0.53681, χ² = 2.372	R_p = 0.034, R_wp = 0.024, R_exp = 0.016, R(F²) = 0.53681, χ² = 2.372	R_p = 0.034, R_wp = 0.024, R_exp = 0.016, R(F²) = 0.53681, χ² = 2.372
No. of data points	1684	2528	2528	2528
No. of parameters	14	8	8	8

	(45470_81B_phase_4)	(45470_81B_phase_5)	(45470_81B_phase_6)
Crystal data
Chemical formula	D	D	D₂O
M_r	2.01	2.01	20.03
Crystal system, space group	Orthorhombic, Pncn	Tetragonal, I4₂d	Trigonal, R3
Temperature (K)	?	?	?
a, b, c (Å)	12.5626 (11), 6.6513 (3), 6.3788 (3)	8.15, 8.15, 4.0	12.8396 (10), 12.8396, 6.1628 (7)
α, β, γ (°)	90, 90, 90	90, 90, 90	90, 90, 120
V (Å³)	533.00 (4)	265.69	879.85 (13)
Z	4	8	36
Radiation type	?, λ = ? Å	?, λ = ? Å	?, λ = ? Å
Specimen shape, size (mm)	?, ? × ? × ?	?, ? × ? × ?	?, ? × ? × ?

Data collection
Diffractometer	?	?	?
Specimen mounting	?	?	?
Data collection mode	?	?	?
Scan method	?	?	?
2θ values (°)	2θ_min = ? 2θ_max = ? 2θ_step = ?	2θ_min = ? 2θ_max = ? 2θ_step = ?	2θ_min = ? 2θ_max = ? 2θ_step = ?

Refinement
R factors and goodness of fit	R_p = 0.034, R_wp = 0.024, R_exp = 0.016, R(F²) = 0.53681, χ² = 2.372	R_p = 0.034, R_wp = 0.024, R_exp = 0.016, R(F²) = 0.53681, χ² = 2.372	R_p = 0.034, R_wp = 0.024, R_exp = 0.016, R(F²) = 0.53681, χ² = 2.372
No. of data points	2528	2528	2528
No. of parameters	8	8	8

Computer programs: GSAS.

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Format		BIBTeX
		EndNote
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		CIF
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		Plain Text