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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.

Supporting information

cif

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

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

Computing details top

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
[Figure 11]
[Figure 12]
[Figure 13]
[Figure 14]
[Figure 15]
[Figure 16]
(G25904_913_AL_ICEIX_phase_1) top
Crystal data top
Dβ = 102.1043 (10)°
Mr = 2.01V = 310.93 (1) Å3
Monoclinic, P21/nZ = 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: full1684 data points
Rp = 0.021Profile 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
Rwp = 0.01914 parameters
Rexp = 0.0120 restraints
R(F2) = 0.19600(Δ/σ)max = 0.04
χ2 = 1.877Background 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
Dβ = 102.1043 (10)°
Mr = 2.01V = 310.93 (1) Å3
Monoclinic, P21/nZ = 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
Rp = 0.021χ2 = 1.877
Rwp = 0.0191684 data points
Rexp = 0.01214 parameters
R(F2) = 0.196000 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
dummy0.00.00.00.025*
(G25904_913_AL_ICEIX_phase_2) top
Crystal data top
Dc = 6.85885 (10) Å
Mr = 2.01V = 899.12 (2) Å3
Orthorhombic, PbcaZ = 4
a = 18.8679 (2) Å? radiation, λ = ? Å
b = 6.94772 (9) Å?; ?, ?; ? × ?; ? mm
Data collection top
Refinement top
Least-squares matrix: full1684 data points
Rp = 0.021Profile 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
Rwp = 0.01914 parameters
Rexp = 0.0120 restraints
R(F2) = 0.19600(Δ/σ)max = 0.04
χ2 = 1.877Background 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
Dc = 6.85885 (10) Å
Mr = 2.01V = 899.12 (2) Å3
Orthorhombic, PbcaZ = 4
a = 18.8679 (2) Å? radiation, λ = ? Å
b = 6.94772 (9) Å?; ?, ?; ? × ?; ? mm
Data collection top
Refinement top
Rp = 0.021χ2 = 1.877
Rwp = 0.0191684 data points
Rexp = 0.01214 parameters
R(F2) = 0.196000 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
dummy0.00.00.00.025*
(G25904_913_AL_ICEIX_phase_3) top
Crystal data top
D2OV = 886.99 (2) Å3
Mr = 20.03Z = 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: full1684 data points
Rp = 0.021Profile 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
Rwp = 0.01914 parameters
Rexp = 0.0120 restraints
R(F2) = 0.19600(Δ/σ)max = 0.04
χ2 = 1.877Background 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
D2OV = 886.99 (2) Å3
Mr = 20.03Z = 36
Trigonal, R3? radiation, λ = ? Å
a = 12.87078 (12) Å?; ?, ?; ? × ?; ? mm
c = 6.1827 (1) Å
Data collection top
Refinement top
Rp = 0.021χ2 = 1.877
Rwp = 0.0191684 data points
Rexp = 0.01214 parameters
R(F2) = 0.196000 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O10.216370.190550.020850.02*
O20.195330.235190.480440.02*
D10.148650.193050.019530.02*
D20.228880.217220.196530.02*
D30.105980.210620.486970.02*
D40.247510.314060.543130.02*
(G25904_913_AL_ICEIX_phase_4) top
Crystal data top
AlV = 65.79 (1) Å3
Mr = 26.98Z = 4
Cubic, Fm3m? radiation, λ = ? Å
a = 4.03702 (12) Å?; ?, ?; ? × ?; ? mm
Data collection top
Refinement top
Least-squares matrix: full1684 data points
Rp = 0.021Profile 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
Rwp = 0.01914 parameters
Rexp = 0.0120 restraints
R(F2) = 0.19600(Δ/σ)max = 0.04
χ2 = 1.877Background 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
AlV = 65.79 (1) Å3
Mr = 26.98Z = 4
Cubic, Fm3m? radiation, λ = ? Å
a = 4.03702 (12) Å?; ?, ?; ? × ?; ? mm
Data collection top
Refinement top
Rp = 0.021χ2 = 1.877
Rwp = 0.0191684 data points
Rexp = 0.01214 parameters
R(F2) = 0.196000 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Al0.00.00.00.01*
(G25904_913_AL_ICEIX_phase_5) top
Crystal data top
D2OV = 297.79 (1) Å3
Mr = 20.03Z = 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: full1684 data points
Rp = 0.021Profile 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
Rwp = 0.01914 parameters
Rexp = 0.0120 restraints
R(F2) = 0.19600(Δ/σ)max = 0.04
χ2 = 1.877Background 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
D2OV = 297.79 (1) Å3
Mr = 20.03Z = 12
Tetragonal, P41212? radiation, λ = ? Å
a = 6.6748 (3) Å?; ?, ?; ? × ?; ? mm
c = 6.6838 (6) Å
Data collection top
Refinement top
Rp = 0.021χ2 = 1.877
Rwp = 0.0191684 data points
Rexp = 0.01214 parameters
R(F2) = 0.196000 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O10.1130.3110.2870.062*
O20.3970.3970.00.044*
D10.0040.3380.2430.072*
D20.1090.1820.3180.068*
D30.290.3580.1020.047*
(45470_81B_phase_1) top
Crystal data top
D10.00O5V = 218.72 (5) Å3
Mr = 100.13Z = 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: full2528 data points
Rp = 0.034Profile 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
Rwp = 0.0248 parameters
Rexp = 0.0160 restraints
R(F2) = 0.53681(Δ/σ)max = 0.08
χ2 = 2.372Background 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
D10.00O5V = 218.72 (5) Å3
Mr = 100.13Z = 2
Tetragonal, P42/nmc? radiation, λ = ? Å
a = 6.1860 (8) Å?, ? × ? × ? mm
c = 5.7157 (16) Å
Data collection top
Refinement top
Rp = 0.034χ2 = 2.372
Rwp = 0.0242528 data points
Rexp = 0.0168 parameters
R(F2) = 0.536810 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
O10.750.250.750.025*
O20.750.52950.13390.025*
D10.750.46280.01370.025*0.5
D20.750.37030.13650.025*0.5
D30.750.68720.12480.025*0.5
D40.13250.53070.78440.025*0.5
(45470_81B_phase_2) top
Crystal data top
PbV = 118.43 (1) Å3
Mr = 203.97Z = 4
Cubic, Fm3m? radiation, λ = ? Å
a = 4.9108 (2) Å?, ? × ? × ? mm
Data collection top
Refinement top
Least-squares matrix: full2528 data points
Rp = 0.034Profile 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
Rwp = 0.0248 parameters
Rexp = 0.0160 restraints
R(F2) = 0.53681(Δ/σ)max = 0.08
χ2 = 2.372Background 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
PbV = 118.43 (1) Å3
Mr = 203.97Z = 4
Cubic, Fm3m? radiation, λ = ? Å
a = 4.9108 (2) Å?, ? × ? × ? mm
Data collection top
Refinement top
Rp = 0.034χ2 = 2.372
Rwp = 0.0242528 data points
Rexp = 0.0168 parameters
R(F2) = 0.536810 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb0.00.00.00.025*
(45470_81B_phase_3) top
Crystal data top
CWV = 20.70 (1) Å3
Mr = 195.86Z = 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: full2528 data points
Rp = 0.034Profile 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
Rwp = 0.0248 parameters
Rexp = 0.0160 restraints
R(F2) = 0.53681(Δ/σ)max = 0.08
χ2 = 2.372Background 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
CWV = 20.70 (1) Å3
Mr = 195.86Z = 1
Hexagonal, P6m2? radiation, λ = ? Å
a = 2.9016 (3) Å?, ? × ? × ? mm
c = 2.83867 (12) Å
Data collection top
Refinement top
Rp = 0.034χ2 = 2.372
Rwp = 0.0242528 data points
Rexp = 0.0168 parameters
R(F2) = 0.536810 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C0.666670.333330.50.025*
W0.00.00.00.025*
(45470_81B_phase_4) top
Crystal data top
Dc = 6.3788 (3) Å
Mr = 2.01V = 533.00 (4) Å3
Orthorhombic, PncnZ = 4
a = 12.5626 (11) Å? radiation, λ = ? Å
b = 6.6513 (3) Å?, ? × ? × ? mm
Data collection top
Refinement top
Least-squares matrix: full2528 data points
Rp = 0.034Profile 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
Rwp = 0.0248 parameters
Rexp = 0.0160 restraints
R(F2) = 0.53681(Δ/σ)max = 0.08
χ2 = 2.372Background 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
Dc = 6.3788 (3) Å
Mr = 2.01V = 533.00 (4) Å3
Orthorhombic, PncnZ = 4
a = 12.5626 (11) Å? radiation, λ = ? Å
b = 6.6513 (3) Å?, ? × ? × ? mm
Data collection top
Refinement top
Rp = 0.034χ2 = 2.372
Rwp = 0.0242528 data points
Rexp = 0.0168 parameters
R(F2) = 0.536810 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
dummy0.00.00.00.025*
(45470_81B_phase_5) top
Crystal data top
DV = 265.69 Å3
Mr = 2.01Z = 8
Tetragonal, I42d? radiation, λ = ? Å
a = 8.15 Å?, ? × ? × ? mm
c = 4.0 Å
Data collection top
Refinement top
Least-squares matrix: full2528 data points
Rp = 0.034Profile 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
Rwp = 0.0248 parameters
Rexp = 0.0160 restraints
R(F2) = 0.53681(Δ/σ)max = 0.08
χ2 = 2.372Background 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
DV = 265.69 Å3
Mr = 2.01Z = 8
Tetragonal, I42d? radiation, λ = ? Å
a = 8.15 Å?, ? × ? × ? mm
c = 4.0 Å
Data collection top
Refinement top
Rp = 0.034χ2 = 2.372
Rwp = 0.0242528 data points
Rexp = 0.0168 parameters
R(F2) = 0.536810 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
dummy0.00.00.00.025*
(45470_81B_phase_6) top
Crystal data top
D2OV = 879.85 (13) Å3
Mr = 20.03Z = 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: full2528 data points
Rp = 0.034Profile 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
Rwp = 0.0248 parameters
Rexp = 0.0160 restraints
R(F2) = 0.53681(Δ/σ)max = 0.08
χ2 = 2.372Background 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
D2OV = 879.85 (13) Å3
Mr = 20.03Z = 36
Trigonal, R3? radiation, λ = ? Å
a = 12.8396 (10) Å?, ? × ? × ? mm
c = 6.1628 (7) Å
Data collection top
Refinement top
Rp = 0.034χ2 = 2.372
Rwp = 0.0242528 data points
Rexp = 0.0168 parameters
R(F2) = 0.536810 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O10.216370.190550.020850.02*
O20.195330.235190.480440.02*
D10.148650.193050.019530.02*
D20.228880.217220.196530.02*
D30.105980.210620.486970.02*
D40.247510.314060.543130.02*

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 formulaDDD2OAl
Mr2.012.0120.0326.98
Crystal system, space groupMonoclinic, P21/nOrthorhombic, PbcaTrigonal, R3Cubic, 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), 9090, 90, 9090, 90, 12090, 90, 90
V3)310.93 (1)899.12 (2)886.99 (2)65.79 (1)
Z24364
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 (°)2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?
Refinement
R factors and goodness of fitRp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877Rp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877Rp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877Rp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877
No. of data points1684168416841684
No. of parameters14141414


(G25904_913_AL_ICEIX_phase_5)(45470_81B_phase_1)(45470_81B_phase_2)(45470_81B_phase_3)
Crystal data
Chemical formulaD2OD10.00O5PbCW
Mr20.03100.13203.97195.86
Crystal system, space groupTetragonal, P41212Tetragonal, P42/nmcCubic, Fm3mHexagonal, 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, 4.910752.9016 (3), 2.90156, 2.83867 (12)
α, β, γ (°)90, 90, 9090, 90, 9090, 90, 9090, 90, 120
V3)297.79 (1)218.72 (5)118.43 (1)20.70 (1)
Z12241
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 (°)2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?
Refinement
R factors and goodness of fitRp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372
No. of data points1684252825282528
No. of parameters14888


(45470_81B_phase_4)(45470_81B_phase_5)(45470_81B_phase_6)
Crystal data
Chemical formulaDDD2O
Mr2.012.0120.03
Crystal system, space groupOrthorhombic, PncnTetragonal, I42dTrigonal, R3
Temperature (K)???
a, b, c (Å)12.5626 (11), 6.6513 (3), 6.3788 (3)8.15, 8.15, 4.012.8396 (10), 12.8396, 6.1628 (7)
α, β, γ (°)90, 90, 9090, 90, 9090, 90, 120
V3)533.00 (4)265.69879.85 (13)
Z4836
Radiation type?, λ = ? Å?, λ = ? Å?, λ = ? Å
Specimen shape, size (mm)?, ? × ? × ??, ? × ? × ??, ? × ? × ?
Data collection
Diffractometer???
Specimen mounting???
Data collection mode???
Scan method???
2θ values (°)2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?2θmin = ? 2θmax = ? 2θstep = ?
Refinement
R factors and goodness of fitRp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372
No. of data points252825282528
No. of parameters888

Computer programs: GSAS.

 

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