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Three complete neutron diffraction datasets have been collected for deuterated malonic acid single crystals, DOOC(CD
2)COOD, above (153 K), just below (56 K) and further below (50 K) the low-temperature phase transition (
Tc = 57 K). The structural details obtained for this transition, studied previously solely by spectroscopic and calorimetric techniques, clearly establish its first-order nature. At 153 K, the space group is
,
Z = 2,
Z′ = 1. The molecules are packed as linear chains linked end-to-end by asymmetric hydrogen bonds so that the carboxyl groups form cyclic dimers. The deuterons in the carboxyl links are ordered. Neighboring chains are cross-linked through C—D
O hydrogen bonds. Upon cooling through the transition the cell doubles along the
a axis. Molecules which are equivalent by symmetry above
Tc become independent below
Tc owing to conformational changes in alternate chains. At 50 K, the space group is
,
Z = 4,
Z′ = 2. Thermal motion analysis, using for all three temperatures the same segmented rigid-body model, reveals a large torsional motion around the one COOD group associated with the conformational change. Refinements were carried out on all three datasets with an anharmonic structural model, including higher-order displacement tensors (Gram–Charlier expansion up to fourth order). Only atoms involved in torsional motion exhibit a significant anharmonic component which increases with temperature.
Supporting information
CCDC references: 685159; 685160; 685161
Program(s) used to refine structure: UPALS(Lundgren,82)&NOOT(Craven et al.,91) for (50K); UPALS (Lundgren,82)& NOOT(Craven et al.,91) for (56K); UPALS(Lundgren,'82)& NOOT(Craven et al.,91) for 153K. For all compounds, molecular graphics: DIAMOND (Brandenburg, 2006).
Crystal data top
C3D4O4 | Z = 4 |
Mr = 108.03 | Dx = 1.758 Mg m−3 |
Triclinic, P1 | Neutron radiation, λ = 1.1588 Å |
a = 10.663 (4) Å | Cell parameters from 32 reflections |
b = 5.142 (2) Å | θ = 29–35° |
c = 11.234 (2) Å | µ = 0.02 mm−1 |
α = 103.39 (3)° | T = 50 K |
β = 136.81 (2)° | Prism, colourless |
γ = 85.19 (3)° | 3.0 × 2.4 × 2.0 mm |
V = 406.8 (3) Å3 | |
Data collection top
Four-circle diffractometers H6S | 2307 independent reflections |
Radiation source: steady-state reactor | Rint = 0.019 |
Ge 022 monochromator | θmax = 54.2°, θmin = 1.8° |
θ–2θ scans | h = −14→14 |
Absorption correction: analytical Templeton & Templeton, 1973 | k = −7→7 |
Tmin = 0.95, Tmax = 0.97 | l = −15→15 |
2653 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[s2(Fo2) + (0.02(Fo2)2 + 0.05] |
wR(F2) = 0.052 | |
S = 1.53 | Δρmax = 0.27 e Å−3 |
2300 reflections | Δρmin = −0.40 e Å−3 |
208 parameters | Extinction correction: Becker & Coppens |
0 restraints | Extinction coefficient: 0.102 (2) |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
C3D4O4 | γ = 85.19 (3)° |
Mr = 108.03 | V = 406.8 (3) Å3 |
Triclinic, P1 | Z = 4 |
a = 10.663 (4) Å | Neutron radiation, λ = 1.1588 Å |
b = 5.142 (2) Å | µ = 0.02 mm−1 |
c = 11.234 (2) Å | T = 50 K |
α = 103.39 (3)° | 3.0 × 2.4 × 2.0 mm |
β = 136.81 (2)° | |
Data collection top
Four-circle diffractometers H6S | 2653 measured reflections |
Absorption correction: analytical Templeton & Templeton, 1973 | 2307 independent reflections |
Tmin = 0.95, Tmax = 0.97 | Rint = 0.019 |
Refinement top
wR(F2) = 0.052 | 0 restraints |
S = 1.53 | Δρmax = 0.27 e Å−3 |
2300 reflections | Δρmin = −0.40 e Å−3 |
208 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C0A | 0.03930 (9) | 0.11744 (12) | 0.23688 (8) | 0.0148 (2) | |
C1A | 0.03043 (8) | 0.29771 (12) | 0.35716 (8) | 0.0111 (2) | |
C2A | 0.01821 (8) | 0.27417 (12) | 0.12644 (8) | 0.0122 (2) | |
O11A | 0.03285 (10) | 0.54168 (14) | 0.37702 (9) | 0.0169 (2) | |
O12A | 0.02100 (10) | 0.16141 (14) | 0.43609 (10) | 0.0218 (2) | |
O21A | 0.14782 (10) | 0.35536 (17) | 0.16073 (11) | 0.0318 (2) | |
O22A | −0.15367 (10) | 0.31321 (16) | −0.01041 (10) | 0.0236 (2) | |
D12A | 0.01040 (13) | 0.28907 (17) | 0.51169 (12) | 0.0334 (2) | |
D21A | −0.15710 (12) | 0.43044 (18) | −0.07171 (12) | 0.0336 (2) | |
D01A | 0.17288 (13) | 0.04118 (19) | 0.32179 (12) | 0.0487 (2) | |
D02A | −0.07034 (13) | −0.05104 (17) | 0.15137 (12) | 0.0314 (2) | |
C0B | 0.55989 (9) | 0.12874 (12) | 0.25322 (8) | 0.0142 (2) | |
C1B | 0.54465 (8) | 0.30473 (12) | 0.36932 (8) | 0.0119 (2) | |
C2B | 0.53347 (8) | 0.28585 (12) | 0.13977 (8) | 0.0113 (2) | |
O11B | 0.52689 (10) | 0.54377 (14) | 0.37533 (9) | 0.0192 (2) | |
O12B | 0.55247 (11) | 0.17081 (14) | 0.46038 (10) | 0.0239 (2) | |
O21B | 0.65638 (10) | 0.44400 (15) | 0.19758 (10) | 0.0213 (2) | |
O22B | 0.36557 (10) | 0.23937 (15) | −0.02523 (10) | 0.0186 (2) | |
D12B | 0.52762 (12) | 0.28434 (17) | 0.52534 (12) | 0.0408 (2) | |
D21B | 0.35396 (12) | 0.35973 (18) | −0.09028 (12) | 0.0331 (2) | |
D01B | 0.69712 (13) | 0.06327 (18) | 0.34140 (12) | 0.0488 (2) | |
D02B | 0.45644 (17) | −0.04789 (17) | 0.17098 (12) | 0.0248 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C0A | 0.0091 (3) | 0.0058 (2) | 0.0074 (2) | 0.0015 (2) | 0.0071 (2) | 0.0016 (2) |
C1A | 0.0067 (2) | 0.0051 (2) | 0.0057 (2) | 0.0004 (2) | 0.0053 (2) | 0.0010 (2) |
C2A | 0.0065 (3) | 0.0067 (2) | 0.0057 (2) | 0.0010 (2) | 0.0050 (2) | 0.0013 (2) |
O11A | 0.0096 (3) | 0.0052 (3) | 0.0077 (3) | 0.0009 (2) | 0.0072 (3) | 0.0010 (2) |
O12A | 0.0140 (3) | 0.0057 (3) | 0.0097 (3) | 0.0016 (2) | 0.0105 (3) | 0.0021 (2) |
O21A | 0.0076 (3) | 0.0184 (3) | 0.0120 (3) | 0.0029 (2) | 0.0072 (3) | 0.0089 (3) |
O22A | 0.0072 (3) | 0.0143 (3) | 0.0087 (3) | 0.0004 (2) | 0.0051 (3) | 0.0052 (2) |
D12A | 0.0219 (5) | 0.0134 (4) | 0.0167 (4) | 0.0019 (3) | 0.0168 (4) | 0.0020 (3) |
D21A | 0.0157 (4) | 0.0210 (5) | 0.0156 (5) | 0.0033 (3) | 0.0109 (4) | 0.0094 (3) |
D01A | 0.0181 (5) | 0.0207 (5) | 0.0192 (5) | 0.0105 (3) | 0.0150 (4) | 0.0108 (3) |
D02A | 0.0222 (5) | 0.0121 (4) | 0.0175 (5) | −0.0053 (3) | 0.0153 (4) | −0.0019 (3) |
C0B | 0.0083 (2) | 0.0061 (2) | 0.0063 (2) | 0.0014 (2) | 0.0060 (2) | 0.0015 (2) |
C1B | 0.0065 (2) | 0.0056 (2) | 0.0057 (2) | 0.0009 (2) | 0.0051 (2) | 0.0012 (2) |
C2B | 0.0069 (2) | 0.0063 (2) | 0.0060 (2) | 0.0005 (2) | 0.0055 (2) | 0.0010 (2) |
O11B | 0.0102 (3) | 0.0058 (3) | 0.0087 (3) | 0.0017 (2) | 0.0080 (3) | 0.0019 (2) |
O12B | 0.0145 (3) | 0.0067 (3) | 0.0110 (3) | 0.0033 (2) | 0.0116 (3) | 0.0036 (2) |
O21B | 0.0071 (3) | 0.0128 (3) | 0.0079 (3) | −0.0003 (2) | 0.0048 (2) | 0.0038 (2) |
O22B | 0.0076 (3) | 0.0119 (3) | 0.0070 (3) | −0.0013 (2) | 0.0045 (3) | 0.0027 (2) |
D12B | 0.0211 (5) | 0.0151 (4) | 0.0167 (4) | 0.0039 (3) | 0.0165 (4) | 0.0041 (3) |
D21B | 0.0157 (4) | 0.0201 (5) | 0.0130 (4) | 0.0006 (3) | 0.0095 (4) | 0.0070 (3) |
D01B | 0.0181 (5) | 0.0212 (5) | 0.0187 (5) | 0.0093 (3) | 0.0146 (4) | 0.0097 (3) |
D02B | 0.0229 (5) | 0.0120 (4) | 0.0173 (5) | −0.0046 (3) | 0.0155 (4) | −0.0010 (3) |
Crystal data top
C3D4O4 | Z = 4 |
Mr = 108.03 | Dx = 1.747 Mg m−3 |
Triclinic, P1 | Neutron radiation, λ = 1.0411 Å |
a = 10.675 (1) Å | Cell parameters from 32 reflections |
b = 5.152 (1) Å | θ = 29–35° |
c = 11.238 (1) Å | µ = 0.02 mm−1 |
α = 103.35 (1)° | T = 56 K |
β = 136.68 (1)° | Prism, colourless |
γ = 85.07 (1)° | 3.0 × 2.4 × 2.0 mm |
V = 409.45 (13) Å3 | |
Data collection top
Four-circle diffractometers H6M | 3203 independent reflections |
Radiation source: steady-state reactor | Rint = 0.022 |
Be 002 monochromator | θmax = 55.3°, θmin = 1.8° |
θ–2θ scans | h = −14→14 |
Absorption correction: analytical Templeton & Templeton, 1973 | k = −7→7 |
Tmin = 0.95, Tmax = 0.97 | l = −15→15 |
4641 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[s2(Fo2) + (0.02(Fo2))2] |
wR(F2) = 0.049 | |
S = 1.02 | Δρmax = 0.45 e Å−3 |
3205 reflections | Δρmin = −0.50 e Å−3 |
208 parameters | Extinction correction: Becker & Coppens |
0 restraints | Extinction coefficient: 0.103 (3) |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
C3D4O4 | γ = 85.07 (1)° |
Mr = 108.03 | V = 409.45 (13) Å3 |
Triclinic, P1 | Z = 4 |
a = 10.675 (1) Å | Neutron radiation, λ = 1.0411 Å |
b = 5.152 (1) Å | µ = 0.02 mm−1 |
c = 11.238 (1) Å | T = 56 K |
α = 103.35 (1)° | 3.0 × 2.4 × 2.0 mm |
β = 136.68 (1)° | |
Data collection top
Four-circle diffractometers H6M | 4641 measured reflections |
Absorption correction: analytical Templeton & Templeton, 1973 | 3203 independent reflections |
Tmin = 0.95, Tmax = 0.97 | Rint = 0.022 |
Refinement top
wR(F2) = 0.049 | 0 restraints |
S = 1.02 | Δρmax = 0.45 e Å−3 |
3205 reflections | Δρmin = −0.50 e Å−3 |
208 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C0A | 0.04205 (7) | 0.11896 (9) | 0.23879 (6) | 0.0194 (3) | |
C1A | 0.03183 (6) | 0.29815 (9) | 0.35818 (6) | 0.0138 (2) | |
C2A | 0.02027 (6) | 0.27620 (9) | 0.12820 (6) | 0.0165 (2) | |
O11A | 0.03222 (8) | 0.54172 (11) | 0.37671 (7) | 0.0188 (3) | |
O12A | 0.02349 (8) | 0.16217 (11) | 0.43784 (8) | 0.0233 (4) | |
O21A | 0.15011 (8) | 0.36856 (15) | 0.16683 (9) | 0.0406 (7) | |
O22A | −0.15193 (8) | 0.30361 (14) | −0.01291 (8) | 0.0231 (4) | |
D12A | 0.01138 (10) | 0.28128 (14) | 0.51244 (9) | 0.0360 (5) | |
D21A | −0.15632 (10) | 0.42136 (16) | −0.07479 (10) | 0.0391 (6) | |
D01A | 0.17582 (11) | 0.04376 (16) | 0.32382 (10) | 0.0533 (8) | |
D02A | −0.06682 (11) | −0.05039 (14) | 0.15360 (10) | 0.0295 (6) | |
C0B | 0.55955 (7) | 0.12864 (9) | 0.25266 (6) | 0.0168 (2) | |
C1B | 0.54391 (6) | 0.30411 (9) | 0.36861 (6) | 0.0154 (2) | |
C2B | 0.53307 (6) | 0.28594 (9) | 0.13935 (6) | 0.0135 (2) | |
O11B | 0.52746 (8) | 0.54355 (11) | 0.37560 (7) | 0.0228 (3) | |
O12B | 0.54962 (8) | 0.16994 (11) | 0.45802 (8) | 0.0284 (4) | |
O21B | 0.65628 (8) | 0.43881 (12) | 0.19565 (8) | 0.0169 (3) | |
O22B | 0.36412 (8) | 0.24381 (12) | −0.02455 (7) | 0.0148 (2) | |
D12B | 0.52587 (10) | 0.28417 (14) | 0.52391 (10) | 0.0413 (7) | |
D21B | 0.35296 (10) | 0.36400 (10) | −0.08948 (9) | 0.0308 (5) | |
D01B | 0.69645 (10) | 0.06306 (15) | 0.34061 (10) | 0.0454 (7) | |
D02B | 0.45652 (11) | −0.04779 (14) | 0.17057 (10) | 0.0272 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C0A | 0.0125 (2) | 0.0079 (2) | 0.0092 (2) | 0.0021 (2) | 0.0092 (2) | 0.0030 (1) |
C1A | 0.0087 (2) | 0.0071 (2) | 0.0068 (2) | 0.0009 (1) | 0.0063 (1) | 0.0023 (1) |
C2A | 0.0097 (2) | 0.0091 (2) | 0.0077 (2) | 0.0015 (1) | 0.0072 (2) | 0.0010 (2) |
O11A | 0.0125 (2) | 0.0073 (2) | 0.0098 (2) | 0.0014 (2) | 0.0094 (2) | 0.0027 (2) |
O12A | 0.0161 (2) | 0.0077 (2) | 0.0109 (2) | 0.0022 (2) | 0.0118 (2) | 0.0036 (2) |
O21A | 0.0102 (2) | 0.0290 (3) | 0.0176 (3) | 0.0058 (2) | 0.0101 (2) | 0.0166 (2) |
O22A | 0.0096 (2) | 0.0214 (3) | 0.0106 (2) | −0.0004 (2) | 0.0056 (2) | 0.0086 (2) |
D12A | 0.0244 (4) | 0.0155 (3) | 0.0181 (3) | 0.0028 (2) | 0.0183 (3) | 0.0040 (2) |
D21A | 0.0176 (3) | 0.0271 (4) | 0.0173 (3) | 0.0031 (2) | 0.0117 (3) | 0.0128 (3) |
D01A | 0.0233 (4) | 0.0244 (4) | 0.0224 (4) | 0.0125 (2) | 0.0187 (3) | 0.0134 (3) |
D02A | 0.0283 (4) | 0.0152 (3) | 0.0198 (4) | −0.0054 (2) | 0.0186 (3) | −0.0007 (2) |
C0B | 0.0113 (2) | 0.0077 (2) | 0.0082 (2) | 0.0013 (1) | 0.0081 (2) | 0.0023 (1) |
C1B | 0.0088 (2) | 0.0079 (2) | 0.0073 (2) | 0.0015 (1) | 0.0066 (2) | 0.0030 (1) |
C2B | 0.0085 (2) | 0.0087 (2) | 0.0066 (2) | 0.0004 (1) | 0.0060 (2) | 0.0021 (1) |
O11B | 0.0139 (2) | 0.0080 (2) | 0.0115 (2) | 0.0026 (2) | 0.0110 (2) | 0.0039 (2) |
O12B | 0.0171 (2) | 0.0090 (2) | 0.0130 (2) | 0.0041 (2) | 0.0134 (2) | 0.0055 (2) |
O21B | 0.0087 (2) | 0.0150 (2) | 0.0084 (2) | −0.0010 (2) | 0.0055 (2) | 0.0048 (2) |
O22B | 0.0094 (2) | 0.0133 (2) | 0.0069 (2) | −0.0013 (2) | 0.0049 (2) | 0.0038 (2) |
D12B | 0.0252 (4) | 0.0171 (3) | 0.0197 (3) | 0.0052 (2) | 0.0196 (3) | 0.0063 (2) |
D21B | 0.0179 (3) | 0.0217 (4) | 0.0143 (3) | 0.0008 (2) | 0.0107 (3) | 0.0079 (2) |
D01B | 0.0198 (3) | 0.0233 (4) | 0.0199 (3) | 0.0098 (2) | 0.0156 (3) | 0.0111 (2) |
D02B | 0.0252 (4) | 0.0144 (3) | 0.0186 (3) | −0.0050 (2) | 0.0166 (3) | 0.0000 (2) |
Crystal data top
C3D4O4 | Z = 2 |
Mr = 108.03 | Dx = 1.733 Mg m−3 |
Triclinic, P1 | Neutron radiation, λ = 1.1588 Å |
a = 5.333 (2) Å | Cell parameters from 32 reflections |
b = 5.158 (2) Å | θ = 29–35° |
c = 11.250 (2) Å | µ = 0.02 mm−1 |
α = 103.33 (3)° | T = 153 K |
β = 136.40 (2)° | Prism, colourless |
γ = 84.76 (3)° | 3.0 × 2.4 × 2.0 mm |
V = 206.34 (15) Å3 | |
Data collection top
Four-circle diffractometers H6S | 1169 independent reflections |
Radiation source: steady-state reactor | Rint = 0.011 |
Ge 022 monochromator | θmax = 54.2°, θmin = 1.8° |
θ–2θ scans | h = −7→7 |
Absorption correction: analytical Templeton & Templeton, 1973 | k = −7→7 |
Tmin = 0.95, Tmax = 0.97 | l = −15→15 |
1345 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.020 (Fo2))2 + 514] |
wR(F2) = 0.040 | |
S = 1.04 | Δρmax = 0.53 e Å−3 |
1177 reflections | Δρmin = −0.60 e Å−3 |
105 parameters | Extinction correction: Becker & Coppens |
0 restraints | Extinction coefficient: 0.125 (3) |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
C3D4O4 | γ = 84.76 (3)° |
Mr = 108.03 | V = 206.34 (15) Å3 |
Triclinic, P1 | Z = 2 |
a = 5.333 (2) Å | Neutron radiation, λ = 1.1588 Å |
b = 5.158 (2) Å | µ = 0.02 mm−1 |
c = 11.250 (2) Å | T = 153 K |
α = 103.33 (3)° | 3.0 × 2.4 × 2.0 mm |
β = 136.40 (2)° | |
Data collection top
Four-circle diffractometers H6S | 1345 measured reflections |
Absorption correction: analytical Templeton & Templeton, 1973 | 1169 independent reflections |
Tmin = 0.95, Tmax = 0.97 | Rint = 0.011 |
Refinement top
wR(F2) = 0.040 | 0 restraints |
S = 1.04 | Δρmax = 0.53 e Å−3 |
1177 reflections | Δρmin = −0.60 e Å−3 |
105 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C0 | 0.60455 (14) | 0.12563 (10) | 0.24685 (7) | 0.0309 (5) | |
C1 | 0.57591 (13) | 0.30175 (10) | 0.36341 (6) | 0.0247 (4) | |
C2 | 0.55587 (14) | 0.28324 (10) | 0.13513 (7) | 0.0255 (4) | |
O11 | 0.55832 (17) | 0.54299 (12) | 0.37553 (8) | 0.0362 (6) | |
O12 | 0.5723 (5) | 0.1654 (4) | 0.4458 (3) | 0.0531 (8) | |
O21 | 0.8066 (5) | 0.4133 (4) | 0.1845 (3) | 0.0436 (7) | |
O22 | 0.2170 (5) | 0.2676 (5) | −0.0190 (3) | 0.0343 (6) | |
D12 | 0.5371 (2) | 0.28112 (18) | 0.51686 (12) | 0.0552 (8) | |
D21 | 0.1988 (2) | 0.3852 (2) | −0.08380 (13) | 0.0451 (7) | |
D01 | 0.8758 (2) | 0.05620 (15) | 0.33327 (10) | 0.0742 (10) | |
D02 | 0.3974 (2) | −0.04627 (14) | 0.16512 (10) | 0.0431 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C0 | 0.0195 (2) | 0.0123 (2) | 0.0155 (2) | 0.0034 (2) | 0.0145 (2) | 0.0043 (2) |
C1 | 0.0136 (2) | 0.0114 (2) | 0.0126 (2) | 0.0025 (2) | 0.0106 (2) | 0.0043 (2) |
C2 | 0.0152 (2) | 0.0136 (2) | 0.0126 (2) | 0.0017 (2) | 0.0112 (2) | 0.0035 (2) |
O11 | 0.0207 (3) | 0.0115 (2) | 0.0184 (3) | 0.0035 (2) | 0.0167 (3) | 0.0047 (2) |
O12 | 0.0285 (3) | 0.0131 (3) | 0.0215 (3) | 0.0055 (2) | 0.0220 (3) | 0.0070 (2) |
O21 | 0.0145 (3) | 0.0379 (4) | 0.0210 (3) | 0.0019 (3) | 0.0110 (2) | 0.0171 (3) |
O22 | 0.0172 (3) | 0.0313 (3) | 0.0154 (3) | −0.0051 (3) | 0.0082 (3) | 0.0094 (3) |
D12 | 0.0337 (5) | 0.0204 (4) | 0.0268 (4) | 0.0055 (3) | 0.0258 (4) | 0.0076 (3) |
D21 | 0.0239 (4) | 0.0374 (5) | 0.0211 (4) | −0.0013 (3) | 0.0135 (3) | 0.0123 (3) |
D01 | 0.0318 (5) | 0.0314 (4) | 0.0325 (4) | 0.0177 (3) | 0.0266 (4) | 0.0188 (3) |
D02 | 0.0410 (5) | 0.0197 (4) | 0.0285 (4) | −0.0066 (3) | 0.0269 (4) | −0.0006 (3) |
Experimental details
| (50K) | (56K) | (153K) |
Crystal data |
Chemical formula | C3D4O4 | C3D4O4 | C3D4O4 |
Mr | 108.03 | 108.03 | 108.03 |
Crystal system, space group | Triclinic, P1 | Triclinic, P1 | Triclinic, P1 |
Temperature (K) | 50 | 56 | 153 |
a, b, c (Å) | 10.663 (4), 5.142 (2), 11.234 (2) | 10.675 (1), 5.152 (1), 11.238 (1) | 5.333 (2), 5.158 (2), 11.250 (2) |
α, β, γ (°) | 103.39 (3), 136.81 (2), 85.19 (3) | 103.35 (1), 136.68 (1), 85.07 (1) | 103.33 (3), 136.40 (2), 84.76 (3) |
V (Å3) | 406.8 (3) | 409.45 (13) | 206.34 (15) |
Z | 4 | 4 | 2 |
Radiation type | Neutron, λ = 1.1588 Å | Neutron, λ = 1.0411 Å | Neutron, λ = 1.1588 Å |
µ (mm−1) | 0.02 | 0.02 | 0.02 |
Crystal size (mm) | 3.0 × 2.4 × 2.0 | 3.0 × 2.4 × 2.0 | 3.0 × 2.4 × 2.0 |
|
Data collection |
Diffractometer | Four-circle diffractometers H6S | Four-circle diffractometers H6M | Four-circle diffractometers H6S |
Absorption correction | Analytical Templeton & Templeton, 1973 | Analytical Templeton & Templeton, 1973 | Analytical Templeton & Templeton, 1973 |
Tmin, Tmax | 0.95, 0.97 | 0.95, 0.97 | 0.95, 0.97 |
No. of measured, independent and observed reflections | 2653, 2307, ? [I > 2σ(I)] | 4641, 3203, ? [ > 0*σ(I)] | 1345, 1169, ? [ > 0*σ(I)] |
Rint | 0.019 | 0.022 | 0.011 |
(sin θ/λ)max (Å−1) | 0.700 | 0.790 | 0.700 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, 0.052, 1.53 | ?, 0.049, 1.02 | ?, 0.040, 1.04 |
No. of reflections | 2300 | 3205 | 1177 |
No. of parameters | 208 | 208 | 105 |
Δρmax, Δρmin (e Å−3) | 0.27, −0.40 | 0.45, −0.50 | 0.53, −0.60 |
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