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
| 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 |
(G25904_913_AL_ICEIX_phase_1)
top
Crystal data top
D | β = 102.1043 (10)° |
Mr = 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 | |
Refinement top
Least-squares matrix: full | 1684 data points |
Rp = 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 |
Rwp = 0.019 | 14 parameters |
Rexp = 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)° |
Mr = 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 | |
Refinement top
Rp = 0.021 | χ2 = 1.877 |
Rwp = 0.019 | 1684 data points |
Rexp = 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 | Uiso*/Ueq | |
dummy | 0.0 | 0.0 | 0.0 | 0.025* | |
(G25904_913_AL_ICEIX_phase_2)
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Crystal data top
D | c = 6.85885 (10) Å |
Mr = 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 |
Refinement top
Least-squares matrix: full | 1684 data points |
Rp = 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 |
Rwp = 0.019 | 14 parameters |
Rexp = 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 |
Mr = 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 |
Refinement top
Rp = 0.021 | χ2 = 1.877 |
Rwp = 0.019 | 1684 data points |
Rexp = 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 | Uiso*/Ueq | |
dummy | 0.0 | 0.0 | 0.0 | 0.025* | |
(G25904_913_AL_ICEIX_phase_3)
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Crystal data top
D2O | V = 886.99 (2) Å3 |
Mr = 20.03 | Z = 36 |
Trigonal, R3 | ? radiation, λ = ? Å |
a = 12.87078 (12) Å | ?; ?, ?; ? × ?; ? mm |
c = 6.1827 (1) Å | |
Refinement top
Least-squares matrix: full | 1684 data points |
Rp = 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 |
Rwp = 0.019 | 14 parameters |
Rexp = 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 |
Mr = 20.03 | Z = 36 |
Trigonal, R3 | ? radiation, λ = ? Å |
a = 12.87078 (12) Å | ?; ?, ?; ? × ?; ? mm |
c = 6.1827 (1) Å | |
Refinement top
Rp = 0.021 | χ2 = 1.877 |
Rwp = 0.019 | 1684 data points |
Rexp = 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 | Uiso*/Ueq | |
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 |
Mr = 26.98 | Z = 4 |
Cubic, Fm3m | ? radiation, λ = ? Å |
a = 4.03702 (12) Å | ?; ?, ?; ? × ?; ? mm |
Refinement top
Least-squares matrix: full | 1684 data points |
Rp = 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 |
Rwp = 0.019 | 14 parameters |
Rexp = 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 |
Mr = 26.98 | Z = 4 |
Cubic, Fm3m | ? radiation, λ = ? Å |
a = 4.03702 (12) Å | ?; ?, ?; ? × ?; ? mm |
Refinement top
Rp = 0.021 | χ2 = 1.877 |
Rwp = 0.019 | 1684 data points |
Rexp = 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 | Uiso*/Ueq | |
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 |
Mr = 20.03 | Z = 12 |
Tetragonal, P41212 | ? radiation, λ = ? Å |
a = 6.6748 (3) Å | ?; ?, ?; ? × ?; ? mm |
c = 6.6838 (6) Å | |
Refinement top
Least-squares matrix: full | 1684 data points |
Rp = 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 |
Rwp = 0.019 | 14 parameters |
Rexp = 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 |
Mr = 20.03 | Z = 12 |
Tetragonal, P41212 | ? radiation, λ = ? Å |
a = 6.6748 (3) Å | ?; ?, ?; ? × ?; ? mm |
c = 6.6838 (6) Å | |
Refinement top
Rp = 0.021 | χ2 = 1.877 |
Rwp = 0.019 | 1684 data points |
Rexp = 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 | Uiso*/Ueq | |
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* | |
Crystal data top
D10.00O5 | V = 218.72 (5) Å3 |
Mr = 100.13 | Z = 2 |
Tetragonal, P42/nmc | ? radiation, λ = ? Å |
a = 6.1860 (8) Å | ?, ? × ? × ? mm |
c = 5.7157 (16) Å | |
Refinement top
Least-squares matrix: full | 2528 data points |
Rp = 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 |
Rwp = 0.024 | 8 parameters |
Rexp = 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
D10.00O5 | V = 218.72 (5) Å3 |
Mr = 100.13 | Z = 2 |
Tetragonal, P42/nmc | ? radiation, λ = ? Å |
a = 6.1860 (8) Å | ?, ? × ? × ? mm |
c = 5.7157 (16) Å | |
Refinement top
Rp = 0.034 | χ2 = 2.372 |
Rwp = 0.024 | 2528 data points |
Rexp = 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 | Uiso*/Ueq | 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 |
Crystal data top
Pb | V = 118.43 (1) Å3 |
Mr = 203.97 | Z = 4 |
Cubic, Fm3m | ? radiation, λ = ? Å |
a = 4.9108 (2) Å | ?, ? × ? × ? mm |
Refinement top
Least-squares matrix: full | 2528 data points |
Rp = 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 |
Rwp = 0.024 | 8 parameters |
Rexp = 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 |
Mr = 203.97 | Z = 4 |
Cubic, Fm3m | ? radiation, λ = ? Å |
a = 4.9108 (2) Å | ?, ? × ? × ? mm |
Refinement top
Rp = 0.034 | χ2 = 2.372 |
Rwp = 0.024 | 2528 data points |
Rexp = 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 | Uiso*/Ueq | |
Pb | 0.0 | 0.0 | 0.0 | 0.025* | |
Crystal data top
CW | V = 20.70 (1) Å3 |
Mr = 195.86 | Z = 1 |
Hexagonal, P6m2 | ? radiation, λ = ? Å |
a = 2.9016 (3) Å | ?, ? × ? × ? mm |
c = 2.83867 (12) Å | |
Refinement top
Least-squares matrix: full | 2528 data points |
Rp = 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 |
Rwp = 0.024 | 8 parameters |
Rexp = 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 |
Mr = 195.86 | Z = 1 |
Hexagonal, P6m2 | ? radiation, λ = ? Å |
a = 2.9016 (3) Å | ?, ? × ? × ? mm |
c = 2.83867 (12) Å | |
Refinement top
Rp = 0.034 | χ2 = 2.372 |
Rwp = 0.024 | 2528 data points |
Rexp = 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 | Uiso*/Ueq | |
C | 0.66667 | 0.33333 | 0.5 | 0.025* | |
W | 0.0 | 0.0 | 0.0 | 0.025* | |
Crystal data top
D | c = 6.3788 (3) Å |
Mr = 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 |
Refinement top
Least-squares matrix: full | 2528 data points |
Rp = 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 |
Rwp = 0.024 | 8 parameters |
Rexp = 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 |
Mr = 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 |
Refinement top
Rp = 0.034 | χ2 = 2.372 |
Rwp = 0.024 | 2528 data points |
Rexp = 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 | Uiso*/Ueq | |
dummy | 0.0 | 0.0 | 0.0 | 0.025* | |
Crystal data top
D | V = 265.69 Å3 |
Mr = 2.01 | Z = 8 |
Tetragonal, I42d | ? radiation, λ = ? Å |
a = 8.15 Å | ?, ? × ? × ? mm |
c = 4.0 Å | |
Refinement top
Least-squares matrix: full | 2528 data points |
Rp = 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 |
Rwp = 0.024 | 8 parameters |
Rexp = 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 |
Mr = 2.01 | Z = 8 |
Tetragonal, I42d | ? radiation, λ = ? Å |
a = 8.15 Å | ?, ? × ? × ? mm |
c = 4.0 Å | |
Refinement top
Rp = 0.034 | χ2 = 2.372 |
Rwp = 0.024 | 2528 data points |
Rexp = 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 | Uiso*/Ueq | |
dummy | 0.0 | 0.0 | 0.0 | 0.025* | |
Crystal data top
D2O | V = 879.85 (13) Å3 |
Mr = 20.03 | Z = 36 |
Trigonal, R3 | ? radiation, λ = ? Å |
a = 12.8396 (10) Å | ?, ? × ? × ? mm |
c = 6.1628 (7) Å | |
Refinement top
Least-squares matrix: full | 2528 data points |
Rp = 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 |
Rwp = 0.024 | 8 parameters |
Rexp = 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 |
Mr = 20.03 | Z = 36 |
Trigonal, R3 | ? radiation, λ = ? Å |
a = 12.8396 (10) Å | ?, ? × ? × ? mm |
c = 6.1628 (7) Å | |
Refinement top
Rp = 0.034 | χ2 = 2.372 |
Rwp = 0.024 | 2528 data points |
Rexp = 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 | Uiso*/Ueq | |
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 |
Mr | 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 (°) | 2θmin = ? 2θmax = ? 2θstep = ? | 2θmin = ? 2θmax = ? 2θstep = ? | 2θmin = ? 2θmax = ? 2θstep = ? | 2θmin = ? 2θmax = ? 2θstep = ? |
|
Refinement |
R factors and goodness of fit | Rp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877 | Rp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877 | Rp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877 | Rp = 0.021, Rwp = 0.019, Rexp = 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 | D10.00O5 | Pb | CW |
Mr | 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 (°) | 2θmin = ? 2θmax = ? 2θstep = ? | 2θmin = ? 2θmax = ? 2θstep = ? | 2θmin = ? 2θmax = ? 2θstep = ? | 2θmin = ? 2θmax = ? 2θstep = ? |
|
Refinement |
R factors and goodness of fit | Rp = 0.021, Rwp = 0.019, Rexp = 0.012, R(F2) = 0.19600, χ2 = 1.877 | Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372 | Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372 | Rp = 0.034, Rwp = 0.024, Rexp = 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 |
Mr | 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 (°) | 2θmin = ? 2θmax = ? 2θstep = ? | 2θmin = ? 2θmax = ? 2θstep = ? | 2θmin = ? 2θmax = ? 2θstep = ? |
|
Refinement |
R factors and goodness of fit | Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372 | Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372 | Rp = 0.034, Rwp = 0.024, Rexp = 0.016, R(F2) = 0.53681, χ2 = 2.372 |
No. of data points | 2528 | 2528 | 2528 |
No. of parameters | 8 | 8 | 8 |