The crystal structures of the title compounds were determined with net intensities
I derived
via the background–peak–background procedure. Least-squares optimizations reveal differences between the low-order (0 <
s < 0.7 Å
−1) and high-order (0.7 <
s < 1.0 Å
−1) structure models. The scale factors indicate discrepancies of up to 10% between the low-order and high-order reflection intensities. This observation is compound independent. It reflects the scan-angle-induced truncation error, because the applied scan angle (0.8 + 2.0 tan θ)° underestimates the wavelength dispersion in the monochromated X-ray beam. The observed crystal structures show pseudo-
I-centred sublattices for three of its non-H atoms in the asymmetric unit. Our selection of observed intensities (
I > 3σ) stresses that pseudo-symmetry. Model refinements on individual data sets with (
h +
k +
l) = 2
n and (
h +
k +
l) = 2
n + 1 illustrate the lack of model robustness caused by that pseudo-symmetry. To obtain a better balanced data set and thus a more robust structure we decided to exploit background modelling. We described the background intensities
B(
) with an 11th degree polynomial in θ. This function predicts the local background
b at each position
and defines the counting statistical distribution
P(
B), in which
b serves as average and variance. The observation
R defines
P(
R). This leads to
P(
I) =
P(
R)/
P(
B) and thus
I =
R −
b and σ
2(
I) =
I so that the error σ(
I) is background independent. Within this framework we reanalysed the structure of the copper(II) derivative. Background modelling resulted in a structure model with an improved internal consistency. At the same time the unweighted
R value based on all observations decreased from 10.6 to 8.4%. A redetermination of the structure at 120 K concluded the analysis.
Supporting information
CCDC references: 170324; 170325; 170326
For all compounds, data collection: CAD4_(Enraf-Nonius,_1994); cell refinement: CAD4 (Enraf-Nonius, 1994); data reduction: process_MolEN_(Fair,_1990); program(s) used to solve structure: Patterson and Fourier; program(s) used to refine structure: LSFM MolEN (Fair, 1990); molecular graphics: PLATON (Spek, 2000); software used to prepare material for publication: BTABLE PTABLE CIF IN MolEN (Fair, 1990).
(Cu294K) Copper(II) bis(hydrogenmalonate) dihydrate
top
Crystal data top
C6H10CuO10 | F(000) = 310 |
Mr = 305.68 | Dx = 2.02 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 7.0655 (7) Å | θ = 10.0–23.0° |
b = 7.5017 (8) Å | µ = 2.22 mm−1 |
c = 9.676 (1) Å | T = 294 K |
β = 100.88 (2)° | Prism, blue |
V = 503.6 (2) Å3 | 0.20 × 0.20 × 0.20 mm |
Z = 2 | |
Data collection top
Enraf Nonius CAD4 diffractometer | 4117 reflections with > 0.0σ(I) |
Radiation source: xray tube | Rint = 0 |
Graphite monochromator | θmax = 45.0°, θmin = 1.5° |
ω/2θ scans | h = 0→14 |
Absorption correction: psi scan North et al. (1968) | k = 0→14 |
Tmin = 0.90, Tmax = 1.0 | l = −19→19 |
4333 measured reflections | 3 standard reflections every 120 min |
4117 independent reflections | intensity decay: none |
Refinement top
Refinement on F | 0 constraints |
Least-squares matrix: full | All H-atom parameters refined |
R[F2 > 2σ(F2)] = 0.083 | Weighting scheme based on measured s.u.'s |
wR(F2) = 0.064 | (Δ/σ)max = 0.05 |
S = 4.11 | Δρmax = 1.09 e Å−3 |
4117 reflections | Δρmin = −1.84 e Å−3 |
99 parameters | Absolute structure: 'weight 4Fo2/(σ2(Fo2) + 0.0001 Fo4)' |
0 restraints | |
Crystal data top
C6H10CuO10 | V = 503.6 (2) Å3 |
Mr = 305.68 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 7.0655 (7) Å | µ = 2.22 mm−1 |
b = 7.5017 (8) Å | T = 294 K |
c = 9.676 (1) Å | 0.20 × 0.20 × 0.20 mm |
β = 100.88 (2)° | |
Data collection top
Enraf Nonius CAD4 diffractometer | 4117 reflections with > 0.0σ(I) |
Absorption correction: psi scan North et al. (1968) | Rint = 0 |
Tmin = 0.90, Tmax = 1.0 | 3 standard reflections every 120 min |
4333 measured reflections | intensity decay: none |
4117 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.083 | 0 restraints |
wR(F2) = 0.064 | All H-atom parameters refined |
S = 4.11 | Δρmax = 1.09 e Å−3 |
4117 reflections | Δρmin = −1.84 e Å−3 |
99 parameters | Absolute structure: 'weight 4Fo2/(σ2(Fo2) + 0.0001 Fo4)' |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 1.0000 | 0.0000 | 1.0000 | 0.01851 (9) | |
O1 | 0.7338 (2) | 0.4889 (2) | 0.9444 (2) | 0.0322 (6) | |
O2 | 0.9134 (2) | 0.2475 (1) | 1.0133 (1) | 0.0233 (4) | |
O3 | 0.4451 (2) | −0.0606 (2) | 0.7995 (2) | 0.0279 (5) | |
O4 | 0.7488 (2) | −0.0810 (1) | 0.9062 (1) | 0.0221 (4) | |
Ow | 1.0838 (2) | 0.0884 (2) | 0.7723 (1) | 0.0264 (5) | |
C1 | 0.7609 (2) | 0.3142 (2) | 0.9471 (1) | 0.0176 (4) | |
C3 | 0.5996 (2) | 0.0093 (2) | 0.8578 (2) | 0.0183 (5) | |
C2 | 0.5960 (2) | 0.2097 (2) | 0.8651 (2) | 0.0270 (7) | |
H1w | 1.087 (3) | 0.180 (3) | 0.762 (2) | 0.049 (7)* | |
H2_1 | 0.588 (5) | 0.224 (4) | 0.777 (3) | 0.10 (1)* | |
H2w | 1.198 (4) | 0.054 (3) | 0.778 (3) | 0.048 (7)* | |
H2_2 | 0.480 (6) | 0.229 (5) | 0.914 (4) | 0.13 (1)* | |
H1_1 | 0.8372 | 0.5798 | 1.0037 | 0.0909* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.01515 (8) | 0.01567 (9) | 0.0267 (1) | 0.00193 (7) | −0.00413 (8) | −0.00311 (8) |
O1 | 0.0277 (6) | 0.0240 (5) | 0.0503 (8) | 0.0029 (4) | −0.0054 (6) | −0.0073 (5) |
O2 | 0.0201 (4) | 0.0188 (4) | 0.0335 (5) | 0.0035 (4) | −0.0070 (4) | −0.0057 (4) |
O3 | 0.0172 (4) | 0.0213 (4) | 0.0591 (8) | −0.0011 (4) | −0.0054 (5) | −0.0079 (5) |
O4 | 0.0173 (4) | 0.0188 (4) | 0.0333 (5) | 0.0018 (4) | −0.0036 (4) | −0.0033 (4) |
Ow | 0.0221 (4) | 0.0230 (5) | 0.0361 (5) | −0.0000 (4) | 0.0041 (4) | 0.0015 (4) |
C1 | 0.0169 (4) | 0.0179 (5) | 0.0181 (4) | 0.0010 (4) | 0.0015 (4) | −0.0006 (4) |
C3 | 0.0148 (4) | 0.0178 (5) | 0.0234 (5) | −0.0008 (4) | 0.0008 (4) | −0.0018 (4) |
C2 | 0.0253 (6) | 0.0175 (5) | 0.0444 (8) | −0.0011 (5) | −0.0134 (6) | 0.0016 (6) |
Geometric parameters (Å, º) top
Cu1—O2 | 1.967 (1) | Ow—H1w | 0.70 (2) |
Cu1—O4 | 1.933 (1) | Ow—H2w | 0.84 (3) |
O1—C1 | 1.324 (2) | C1—C2 | 1.501 (2) |
O1—H1_1 | 1.082 (1) | C3—C2 | 1.505 (2) |
O2—C1 | 1.249 (2) | C2—H2_1 | 0.85 (3) |
O3—C3 | 1.246 (2) | C2—H2_2 | 1.03 (4) |
O4—C3 | 1.267 (2) | | |
| | | |
O2—Cu1—O4 | 93.34 (5) | O4—C3—C2 | 122.5 (1) |
C1—O1—H1_1 | 122.2 (1) | C1—C2—C3 | 121.9 (1) |
H1w—Ow—H2w | 104 (2) | C1—C2—H2_1 | 111 (2) |
O1—C1—O2 | 120.9 (1) | C1—C2—H2_2 | 106 (1) |
O1—C1—C2 | 114.3 (1) | C3—C2—H2_1 | 94 (1) |
O2—C1—C2 | 124.8 (1) | C3—C2—H2_2 | 100 (1) |
O3—C3—O4 | 122.6 (1) | H2_1—C2—H2_2 | 122 (3) |
O3—C3—C2 | 114.9 (1) | | |
(Cu120K) Copper(II) Hydrogenmalonate Dihydrate
top
Crystal data top
C6H10CuO10 | F(000) = 310 |
Mr = 305.68 | Dx = 2.07 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 7.019 (2) Å | θ = 10.1–23.0° |
b = 7.472 (2) Å | µ = 2.28 mm−1 |
c = 9.498 (2) Å | T = 120 K |
β = 99.94 (2)° | Prism, blue |
V = 490.7 (4) Å3 | 0.40 × 0.20 × 0.20 mm |
Z = 2 | |
Data collection top
Enraf Nonius CAD4 diffractometer | 2972 reflections with > 3.0σ(I) |
Radiation source: xray tube | Rint = 0 |
Graphite monochromator | θmax = 44.9°, θmin = 1.5° |
ω/2θ scans | h = 0→14 |
Absorption correction: psi scan North et al. (1968) | k = 0→14 |
Tmin = 0.800, Tmax = 1.000 | l = −19→19 |
4248 measured reflections | 3 standard reflections every 120 min |
4248 independent reflections | intensity decay: none |
Refinement top
Refinement on F | 0 constraints |
Least-squares matrix: full | All H-atom parameters refined |
R[F2 > 2σ(F2)] = 0.048 | Weighting scheme based on measured s.u.'s |
wR(F2) = 0.052 | (Δ/σ)max = 0.033 |
S = 3.06 | Δρmax = 1.92 e Å−3 |
2972 reflections | Δρmin = −2.32 e Å−3 |
99 parameters | Absolute structure: 'weight 4Fo2/(σ2(Fo2) + 0.0001Fo4)' |
0 restraints | |
Crystal data top
C6H10CuO10 | V = 490.7 (4) Å3 |
Mr = 305.68 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 7.019 (2) Å | µ = 2.28 mm−1 |
b = 7.472 (2) Å | T = 120 K |
c = 9.498 (2) Å | 0.40 × 0.20 × 0.20 mm |
β = 99.94 (2)° | |
Data collection top
Enraf Nonius CAD4 diffractometer | 2972 reflections with > 3.0σ(I) |
Absorption correction: psi scan North et al. (1968) | Rint = 0 |
Tmin = 0.800, Tmax = 1.000 | 3 standard reflections every 120 min |
4248 measured reflections | intensity decay: none |
4248 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.048 | 0 restraints |
wR(F2) = 0.052 | All H-atom parameters refined |
S = 3.06 | Δρmax = 1.92 e Å−3 |
2972 reflections | Δρmin = −2.32 e Å−3 |
99 parameters | Absolute structure: 'weight 4Fo2/(σ2(Fo2) + 0.0001Fo4)' |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 1.0000 | 0.0000 | 1.0000 | 0.00621 (8) | |
O1 | 0.7352 (2) | 0.4921 (2) | 0.9414 (2) | 0.0157 (5) | |
O2 | 0.9139 (2) | 0.2498 (2) | 1.0125 (1) | 0.0097 (4) | |
O3 | 0.4442 (2) | −0.0620 (2) | 0.7989 (2) | 0.0111 (5) | |
O4 | 0.7487 (2) | −0.0815 (2) | 0.9050 (1) | 0.0091 (4) | |
Ow | 1.0847 (2) | 0.0874 (2) | 0.7724 (1) | 0.0108 (4) | |
C1 | 0.7604 (2) | 0.3165 (2) | 0.9466 (2) | 0.0078 (5) | |
C3 | 0.5985 (2) | 0.0092 (2) | 0.8581 (2) | 0.0083 (5) | |
C2 | 0.5922 (2) | 0.2107 (2) | 0.8688 (2) | 0.0105 (6) | |
H1w | 1.080 (4) | 0.197 (4) | 0.763 (3) | 0.036 (9)* | |
H2_1 | 0.564 (4) | 0.255 (4) | 0.774 (3) | 0.025 (7)* | |
H2w | 1.182 (5) | 0.043 (4) | 0.765 (4) | 0.034 (9)* | |
H2_2 | 0.484 (4) | 0.233 (4) | 0.923 (3) | 0.025 (7)* | |
H1_1 | 0.842 (4) | 0.569 (4) | 0.989 (3) | 0.010 (6)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.00626 (7) | 0.00340 (8) | 0.01128 (9) | 0.0007 (1) | −0.00264 (7) | −0.0009 (1) |
O1 | 0.0157 (5) | 0.0102 (5) | 0.0239 (6) | 0.0008 (5) | −0.0028 (4) | −0.0025 (6) |
O2 | 0.0095 (4) | 0.0065 (4) | 0.0149 (5) | 0.0018 (4) | −0.0037 (4) | −0.0015 (4) |
O3 | 0.0075 (4) | 0.0069 (4) | 0.0269 (6) | −0.0006 (4) | −0.0037 (4) | −0.0040 (5) |
O4 | 0.0079 (4) | 0.0061 (4) | 0.0158 (5) | 0.0010 (4) | −0.0025 (4) | −0.0010 (4) |
Ow | 0.0096 (4) | 0.0076 (4) | 0.0172 (5) | 0.0005 (4) | 0.0003 (4) | 0.0003 (4) |
C1 | 0.0088 (5) | 0.0058 (5) | 0.0094 (5) | 0.0003 (4) | 0.0001 (4) | −0.0003 (5) |
C3 | 0.0084 (4) | 0.0066 (5) | 0.0103 (5) | −0.0010 (6) | 0.0004 (4) | −0.0007 (6) |
C2 | 0.0112 (6) | 0.0052 (5) | 0.0197 (7) | −0.0006 (5) | −0.0053 (5) | 0.0007 (5) |
Geometric parameters (Å, º) top
O1—C1 | 1.324 (2) | C1—C2 | 1.505 (2) |
O1—H1_1 | 0.99 (2) | C3—O3 | 1.249 (2) |
O2—Cu1 | 1.972 (1) | C3—O4 | 1.268 (2) |
O2—C1 | 1.252 (2) | C3—C2 | 1.511 (2) |
O3—C3 | 1.249 (2) | C2—C1 | 1.505 (2) |
O4—Cu1 | 1.936 (1) | C2—C3 | 1.511 (2) |
O4—C3 | 1.268 (2) | C2—H2_1 | 0.95 (3) |
Ow—H1w | 0.82 (3) | C2—H2_2 | 1.00 (3) |
Ow—H2w | 0.77 (3) | Cu1—O2 | 1.972 (1) |
C1—O1 | 1.324 (2) | Cu1—O4 | 1.936 (1) |
C1—O2 | 1.252 (2) | Cu1—Ow | 2.428 (1) |
| | | |
C1—O1—H1_1 | 118 (1) | C1—C2—H2_1 | 107 (1) |
H1w—Ow—H2w | 116 (3) | C1—C2—H2_2 | 104 (1) |
O1—C1—O2 | 120.7 (1) | C3—C2—H2_1 | 106 (1) |
O1—C1—C2 | 114.4 (1) | C3—C2—H2_2 | 103 (1) |
O2—C1—C2 | 124.9 (1) | H2_1—C2—H2_2 | 112 (2) |
O3—C3—O4 | 122.3 (2) | O2—Cu1—O4 | 93.55 (5) |
O3—C3—C2 | 114.9 (1) | O2—Cu1—Ow | 85.64 (5) |
O4—C3—C2 | 122.8 (1) | O4—Cu1—Ow | 90.75 (5) |
C1—C2—C3 | 121.8 (1) | | |
(Mn) Manganese(II) Bis(hydrogenmalonate) Dihydrate
top
Crystal data top
C6H10MnO10 | F(000) = 302 |
Mr = 297.08 | Dx = 2.00 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 7.0909 (7) Å | θ = 12.0–28.0° |
b = 7.3518 (7) Å | µ = 1.39 mm−1 |
c = 9.577 (1) Å | T = 294 K |
β = 99.73 (2)° | Prism, pink |
V = 492.1 (2) Å3 | 0.1 × 0.1 × 0.1 mm |
Z = 2 | |
Data collection top
Enraf Nonius CAD4 diffractometer | 2085 reflections with > 3.0σ(I) |
Radiation source: xray tube | Rint = 0 |
Graphite monochromator | θmax = 49.9°, θmin = 1.5° |
ω/2θ scans | h = 0→15 |
Absorption correction: psi scan North et al. (1968) | k = 0→15 |
Tmin = 0.94, Tmax = 0.999 | l = −20→20 |
5395 measured reflections | 3 standard reflections every 120 min |
5395 independent reflections | intensity decay: none |
Refinement top
Refinement on F | 0 constraints |
Least-squares matrix: full | All H-atom parameters refined |
R[F2 > 2σ(F2)] = 0.060 | Weighting scheme based on measured s.u.'s |
wR(F2) = 0.051 | (Δ/σ)max = 0.018 |
S = 3.06 | Δρmax = 1.66 e Å−3 |
2085 reflections | Δρmin = −1.92 e Å−3 |
99 parameters | Absolute structure: 'weight 4Fo2/(σ2(Fo2) + 0.0001 Fo4)' |
0 restraints | |
Crystal data top
C6H10MnO10 | V = 492.1 (2) Å3 |
Mr = 297.08 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 7.0909 (7) Å | µ = 1.39 mm−1 |
b = 7.3518 (7) Å | T = 294 K |
c = 9.577 (1) Å | 0.1 × 0.1 × 0.1 mm |
β = 99.73 (2)° | |
Data collection top
Enraf Nonius CAD4 diffractometer | 2085 reflections with > 3.0σ(I) |
Absorption correction: psi scan North et al. (1968) | Rint = 0 |
Tmin = 0.94, Tmax = 0.999 | 3 standard reflections every 120 min |
5395 measured reflections | intensity decay: none |
5395 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.060 | 0 restraints |
wR(F2) = 0.051 | All H-atom parameters refined |
S = 3.06 | Δρmax = 1.66 e Å−3 |
2085 reflections | Δρmin = −1.92 e Å−3 |
99 parameters | Absolute structure: 'weight 4Fo2/(σ2(Fo2) + 0.0001 Fo4)' |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 1.0000 | 0.0000 | 1.0000 | 0.0132 (1) | |
O1 | 0.7244 (3) | 0.5026 (3) | 0.9372 (2) | 0.041 (1) | |
O2 | 0.8972 (2) | 0.2574 (3) | 1.0157 (2) | 0.0276 (8) | |
O3 | 0.4367 (2) | −0.0615 (3) | 0.7944 (2) | 0.0292 (8) | |
O4 | 0.7410 (2) | −0.0797 (3) | 0.8926 (2) | 0.0256 (8) | |
Ow | 1.0897 (2) | 0.0889 (2) | 0.8033 (2) | 0.0268 (8) | |
C1 | 0.7477 (3) | 0.3238 (3) | 0.9466 (3) | 0.0214 (9) | |
C3 | 0.5909 (3) | 0.0112 (3) | 0.8533 (2) | 0.0211 (9) | |
C2 | 0.5813 (3) | 0.2144 (3) | 0.8719 (3) | 0.026 (1) | |
H1w | 1.061 (7) | 0.204 (9) | 0.740 (5) | 0.16 (2)* | |
H21 | 0.540 (4) | 0.277 (5) | 0.783 (3) | 0.049 (9)* | |
H2w | 1.207 (5) | 0.044 (5) | 0.784 (4) | 0.06 (1)* | |
H22 | 0.451 (5) | 0.241 (6) | 0.897 (4) | 0.09 (1)* | |
H11 | 0.873 (6) | 0.589 (6) | 0.985 (4) | 0.12 (1)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0110 (1) | 0.0099 (1) | 0.0209 (2) | 0.0009 (2) | −0.0024 (1) | 0.0002 (2) |
O1 | 0.044 (1) | 0.0274 (9) | 0.059 (1) | 0.001 (1) | −0.0039 (9) | −0.003 (1) |
O2 | 0.0270 (8) | 0.0206 (8) | 0.0376 (9) | 0.0045 (7) | −0.0082 (7) | −0.0034 (8) |
O3 | 0.0179 (7) | 0.0269 (8) | 0.052 (1) | −0.0024 (7) | −0.0029 (7) | −0.0098 (8) |
O4 | 0.0207 (7) | 0.0207 (8) | 0.0392 (9) | 0.0015 (7) | −0.0002 (7) | −0.0027 (8) |
Ow | 0.0228 (7) | 0.0245 (8) | 0.0344 (9) | 0.0006 (7) | 0.0038 (7) | 0.0028 (8) |
C1 | 0.0206 (9) | 0.019 (1) | 0.025 (1) | 0.0015 (9) | 0.0029 (8) | −0.0012 (9) |
C3 | 0.0194 (8) | 0.0200 (9) | 0.0240 (9) | −0.001 (1) | 0.0023 (7) | 0.001 (1) |
C2 | 0.022 (1) | 0.019 (1) | 0.041 (1) | 0.0003 (9) | −0.005 (1) | 0.002 (1) |
Geometric parameters (Å, º) top
Mn1—O2 | 2.042 (2) | O4—C3 | 1.260 (3) |
Mn1—O4 | 2.033 (2) | Ow—H1w | 1.04 (6) |
Mn1—Ow | 2.188 (2) | Ow—H2w | 0.94 (3) |
O1—C1 | 1.327 (3) | C1—C2 | 1.505 (3) |
O1—H11 | 1.25 (4) | C3—C2 | 1.507 (4) |
O2—C1 | 1.250 (3) | C2—H21 | 0.97 (3) |
O3—C3 | 1.261 (3) | C2—H22 | 1.01 (4) |
| | | |
O2—Mn1—O4 | 90.07 (7) | O3—C3—C2 | 114.8 (2) |
O2—Mn1—Ow | 86.90 (7) | O4—C3—C2 | 122.9 (2) |
O4—Mn1—Ow | 91.13 (7) | C1—C2—C3 | 122.6 (2) |
C1—O1—H11 | 113 (2) | C1—C2—H21 | 105 (1) |
H1w—Ow—H2w | 105 (3) | C1—C2—H22 | 117 (2) |
O1—C1—O2 | 120.5 (2) | C3—C2—H21 | 112 (1) |
O1—C1—C2 | 114.7 (2) | C3—C2—H22 | 106 (2) |
O2—C1—C2 | 124.7 (2) | H21—C2—H22 | 87 (2) |
O3—C3—O4 | 122.3 (2) | | |
Experimental details
| (Cu294K) | (Cu120K) | (Mn) |
Crystal data |
Chemical formula | C6H10CuO10 | C6H10CuO10 | C6H10MnO10 |
Mr | 305.68 | 305.68 | 297.08 |
Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n | Monoclinic, P21/n |
Temperature (K) | 294 | 120 | 294 |
a, b, c (Å) | 7.0655 (7), 7.5017 (8), 9.676 (1) | 7.019 (2), 7.472 (2), 9.498 (2) | 7.0909 (7), 7.3518 (7), 9.577 (1) |
β (°) | 100.88 (2) | 99.94 (2) | 99.73 (2) |
V (Å3) | 503.6 (2) | 490.7 (4) | 492.1 (2) |
Z | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 2.22 | 2.28 | 1.39 |
Crystal size (mm) | 0.20 × 0.20 × 0.20 | 0.40 × 0.20 × 0.20 | 0.1 × 0.1 × 0.1 |
|
Data collection |
Diffractometer | Enraf Nonius CAD4 diffractometer | Enraf Nonius CAD4 diffractometer | Enraf Nonius CAD4 diffractometer |
Absorption correction | Psi scan North et al. (1968) | Psi scan North et al. (1968) | Psi scan North et al. (1968) |
Tmin, Tmax | 0.90, 1.0 | 0.800, 1.000 | 0.94, 0.999 |
No. of measured, independent and observed reflections | 4333, 4117, 4117 [ > 0.0σ(I)] | 4248, 4248, 2972 [ > 3.0σ(I)] | 5395, 5395, 2085 [ > 3.0σ(I)] |
Rint | 0 | 0 | 0 |
(sin θ/λ)max (Å−1) | 0.994 | 0.994 | 1.077 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.083, 0.064, 4.11 | 0.048, 0.052, 3.06 | 0.060, 0.051, 3.06 |
No. of reflections | 4117 | 2972 | 2085 |
No. of parameters | 99 | 99 | 99 |
H-atom treatment | All H-atom parameters refined | All H-atom parameters refined | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | 1.09, −1.84 | 1.92, −2.32 | 1.66, −1.92 |
Absolute structure | 'weight 4Fo2/(σ2(Fo2) + 0.0001 Fo4)' | 'weight 4Fo2/(σ2(Fo2) + 0.0001Fo4)' | 'weight 4Fo2/(σ2(Fo2) + 0.0001 Fo4)' |