Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536800018791/cf6009sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536800018791/cf6009Isup2.fcf |
CCDC reference: 155842
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.008 Å
- R factor = 0.043
- wR factor = 0.105
- Data-to-parameter ratio = 16.8
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level A:
ABSTM_02 Alert A Test not performed as the _exptl_absorpt_correction_type has not been identified. See test ABSTY_01. ABSTY_01 Alert A The absorption correction should be one of the following * none * analytical * integration * numerical * gaussian * empirical * psi-scan * multi-scan * refdelf * sphere * cylinder
Alert Level C:
PLAT_420 Alert C D-H without acceptor O(1W) - H(12W) ? PLAT_702 Alert C Angle Calc 65.55(15), Rep 65.80(10), Dev. 1.67 Sigma O3 -CE1 -O6W 4.465 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 9 O5 -CU1 -O5 -C5 0.00 0.30 3.555 1.555 1.555 1.555
2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
3 Alert Level C = Please check
The title complex was synthesized from squaric acid, copper chloride and cerium nitrate by using the procedure for the preparation of the lanthanum complex (Bouayad et al., 1992). Two molar equivalents of betaine were then added to the solution of the mixture in an attempt to synthesize the betaine adduct; however, only the title complex separated from solution.
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
[Ce(H2O)6]2[Cu(H2O)4](C4O4)4·2H2O | F(000) = 1098 |
Mr = 1116.23 | Dx = 2.236 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 6.7685 (1) Å | Cell parameters from 8181 reflections |
b = 32.2337 (1) Å | θ = 1.3–28.3° |
c = 8.1730 (1) Å | µ = 3.46 mm−1 |
β = 111.578 (1)° | T = 298 K |
V = 1658.17 (3) Å3 | Plate, yellow |
Z = 2 | 0.32 × 0.18 × 0.04 mm |
Siemens CCD area-detector diffractometer | 4037 independent reflections |
Radiation source: fine-focus sealed tube | 3283 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.075 |
Detector resolution: 8.33 pixels mm-1 | θmax = 28.3°, θmin = 1.3° |
ω scans | h = −9→5 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −42→34 |
Tmin = 0.404, Tmax = 0.874 | l = −9→10 |
11717 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H-atom parameters not refined |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0378P)2] where P = (Fo2 + 2Fc2)/3 |
4037 reflections | (Δ/σ)max = 0.001 |
241 parameters | Δρmax = 1.16 e Å−3 |
0 restraints | Δρmin = −2.62 e Å−3 |
[Ce(H2O)6]2[Cu(H2O)4](C4O4)4·2H2O | V = 1658.17 (3) Å3 |
Mr = 1116.23 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 6.7685 (1) Å | µ = 3.46 mm−1 |
b = 32.2337 (1) Å | T = 298 K |
c = 8.1730 (1) Å | 0.32 × 0.18 × 0.04 mm |
β = 111.578 (1)° |
Siemens CCD area-detector diffractometer | 4037 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3283 reflections with I > 2σ(I) |
Tmin = 0.404, Tmax = 0.874 | Rint = 0.075 |
11717 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 0 restraints |
wR(F2) = 0.105 | H-atom parameters not refined |
S = 1.02 | Δρmax = 1.16 e Å−3 |
4037 reflections | Δρmin = −2.62 e Å−3 |
241 parameters |
x | y | z | Uiso*/Ueq | ||
Ce1 | 0.03834 (4) | 0.157242 (8) | 0.33368 (3) | 0.0103 (1) | |
Cu1 | 0.0000 | 0.0000 | 0.0000 | 0.0149 (2) | |
O1 | 0.2688 (6) | 0.2184 (1) | 0.3781 (5) | 0.024 (1) | |
O2 | 0.6819 (6) | 0.1964 (1) | 0.7230 (5) | 0.022 (1) | |
O3 | 0.7566 (6) | 0.2940 (1) | 0.8134 (5) | 0.021 (1) | |
O4 | 0.3831 (6) | 0.3170 (1) | 0.4447 (5) | 0.021 (1) | |
O5 | 0.1014 (6) | −0.0175 (1) | 0.2464 (5) | 0.020 (1) | |
O6 | 0.0724 (6) | 0.0792 (1) | 0.3433 (5) | 0.017 (1) | |
O7 | 0.3970 (6) | 0.0601 (1) | 0.7457 (5) | 0.024 (1) | |
O8 | 0.3731 (7) | −0.0380 (1) | 0.6492 (5) | 0.023 (1) | |
O1w | −0.0210 (6) | 0.2059 (1) | 0.0606 (5) | 0.024 (1) | |
O2w | 0.3832 (6) | 0.1364 (1) | 0.5774 (5) | 0.023 (1) | |
O3w | 0.2700 (7) | 0.1326 (1) | 0.1717 (5) | 0.022 (1) | |
O4w | −0.2479 (6) | 0.1297 (1) | 0.0479 (5) | 0.022 (1) | |
O5w | −0.2585 (6) | 0.1203 (1) | 0.4127 (5) | 0.022 (1) | |
O6w | 0.0574 (7) | 0.1873 (2) | 0.6301 (5) | 0.036 (1) | |
O7w | −0.2125 (7) | 0.0379 (1) | 0.0340 (5) | 0.023 (1) | |
O8w | 0.2776 (6) | 0.0518 (1) | 0.0558 (5) | 0.022 (1) | |
O9w | −0.1018 (9) | 0.1070 (1) | −0.2044 (6) | 0.042 (1) | |
C1 | 0.4081 (8) | 0.2393 (2) | 0.4942 (7) | 0.016 (1) | |
C2 | 0.5891 (8) | 0.2296 (2) | 0.6506 (7) | 0.015 (1) | |
C3 | 0.6268 (8) | 0.2733 (2) | 0.6887 (7) | 0.016 (1) | |
C4 | 0.4542 (8) | 0.2834 (2) | 0.5248 (7) | 0.014 (1) | |
C5 | 0.1698 (8) | 0.0044 (1) | 0.3830 (6) | 0.011 (1) | |
C6 | 0.1654 (8) | 0.0478 (2) | 0.4274 (7) | 0.013 (1) | |
C7 | 0.3072 (9) | 0.0388 (2) | 0.6108 (7) | 0.016 (1) | |
C8 | 0.2975 (8) | −0.0053 (2) | 0.5667 (6) | 0.014 (1) | |
H1w1 | −0.0359 | 0.1890 | −0.0431 | 0.050* | |
H1w2 | 0.1007 | 0.2241 | 0.0842 | 0.050* | |
H2w1 | 0.4961 | 0.1557 | 0.6411 | 0.050* | |
H2w2 | 0.4043 | 0.1110 | 0.6456 | 0.050* | |
H3w1 | 0.2284 | 0.1040 | 0.1433 | 0.050* | |
H3w2 | 0.2606 | 0.1466 | 0.0632 | 0.050* | |
H4w1 | −0.1948 | 0.1381 | −0.0437 | 0.050* | |
H4w2 | −0.3660 | 0.1480 | 0.0389 | 0.050* | |
H5w1 | −0.2371 | 0.0908 | 0.3996 | 0.060* | |
H5w2 | −0.2181 | 0.1246 | 0.5394 | 0.060* | |
H6w1 | 0.1537 | 0.1704 | 0.7237 | 0.050* | |
H6w2 | −0.0805 | 0.1878 | 0.6410 | 0.050* | |
H7w1 | −0.2825 | 0.0541 | −0.0734 | 0.050* | |
H7w2 | −0.1426 | 0.0568 | 0.1302 | 0.050* | |
H8w1 | 0.2896 | 0.0599 | −0.0549 | 0.050* | |
H8w2 | 0.4205 | 0.0446 | 0.1375 | 0.050* | |
H9w1 | −0.1272 | 0.0770 | −0.1966 | 0.050* | |
H9w2 | −0.1473 | 0.1137 | −0.3296 | 0.050* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ce1 | 0.0108 (2) | 0.0096 (2) | 0.0080 (2) | 0.0006 (1) | 0.0006 (1) | −0.0005 (1) |
Cu1 | 0.0209 (5) | 0.0148 (5) | 0.0067 (4) | 0.0035 (4) | 0.0023 (3) | −0.0004 (3) |
O1 | 0.024 (2) | 0.020 (2) | 0.019 (2) | −0.011 (2) | −0.002 (2) | −0.006 (2) |
O2 | 0.023 (2) | 0.015 (2) | 0.021 (2) | 0.001 (2) | −0.003 (2) | 0.001 (2) |
O3 | 0.023 (2) | 0.024 (2) | 0.014 (2) | −0.013 (2) | 0.004 (2) | −0.007 (2) |
O4 | 0.025 (2) | 0.013 (2) | 0.019 (2) | 0.002 (2) | 0.003 (2) | 0.001 (2) |
O5 | 0.032 (2) | 0.016 (2) | 0.008 (2) | 0.001 (2) | 0.004 (2) | −0.001 (2) |
O6 | 0.021 (2) | 0.008 (2) | 0.017 (2) | 0.004 (2) | 0.002 (2) | 0.003 (1) |
O7 | 0.032 (2) | 0.019 (2) | 0.012 (2) | −0.004 (2) | −0.002 (2) | −0.004 (2) |
O8 | 0.030 (2) | 0.014 (2) | 0.018 (2) | 0.002 (2) | 0.000 (2) | 0.006 (2) |
O1w | 0.030 (2) | 0.024 (2) | 0.014 (2) | −0.004 (2) | 0.004 (2) | 0.000 (2) |
O2w | 0.021 (2) | 0.013 (2) | 0.023 (2) | −0.001 (2) | −0.005 (2) | 0.001 (2) |
O3w | 0.031 (2) | 0.016 (2) | 0.024 (2) | 0.003 (2) | 0.016 (2) | 0.003 (2) |
O4w | 0.024 (2) | 0.025 (2) | 0.012 (2) | 0.002 (2) | 0.001 (2) | 0.000 (2) |
O5w | 0.025 (2) | 0.019 (2) | 0.024 (2) | 0.000 (2) | 0.013 (2) | −0.002 (2) |
O6w | 0.022 (2) | 0.065 (3) | 0.016 (2) | 0.010 (2) | 0.001 (2) | −0.004 (2) |
O7w | 0.035 (2) | 0.018 (2) | 0.016 (2) | 0.005 (2) | 0.009 (2) | −0.003 (2) |
O8w | 0.022 (2) | 0.025 (2) | 0.015 (2) | −0.001 (2) | 0.003 (2) | −0.002 (2) |
O9w | 0.075 (4) | 0.030 (3) | 0.026 (3) | 0.012 (2) | 0.025 (3) | 0.006 (2) |
C1 | 0.015 (3) | 0.021 (3) | 0.011 (2) | −0.005 (2) | 0.004 (2) | −0.003 (2) |
C2 | 0.017 (3) | 0.014 (3) | 0.015 (3) | −0.004 (2) | 0.007 (2) | −0.001 (2) |
C3 | 0.015 (3) | 0.021 (3) | 0.013 (3) | −0.003 (2) | 0.007 (2) | −0.001 (2) |
C4 | 0.017 (3) | 0.016 (3) | 0.011 (3) | −0.003 (2) | 0.006 (2) | −0.002 (2) |
C5 | 0.013 (2) | 0.009 (2) | 0.012 (2) | −0.003 (2) | 0.007 (2) | 0.002 (2) |
C6 | 0.014 (3) | 0.013 (2) | 0.012 (2) | 0.002 (2) | 0.007 (2) | 0.002 (2) |
C7 | 0.020 (3) | 0.019 (3) | 0.009 (2) | −0.002 (2) | 0.006 (2) | 0.000 (2) |
C8 | 0.016 (3) | 0.017 (3) | 0.008 (2) | −0.002 (2) | 0.003 (2) | 0.000 (2) |
Ce1—O1 | 2.456 (4) | C2—C3 | 1.446 (7) |
Ce1—O3i | 2.429 (4) | C3—C4 | 1.454 (7) |
Ce1—O6 | 2.525 (3) | C5—C6 | 1.449 (7) |
Ce1—O1w | 2.635 (4) | C5—C8 | 1.464 (7) |
Ce1—O2w | 2.540 (4) | C6—C7 | 1.481 (7) |
Ce1—O3w | 2.523 (4) | C7—C8 | 1.462 (7) |
Ce1—O4w | 2.582 (4) | O1w—H1w1 | 0.98 |
Ce1—O5w | 2.613 (4) | O1w—H1w2 | 0.97 |
Ce1—O6w | 2.568 (4) | O2w—H2w1 | 0.98 |
Cu1—O5 | 1.957 (4) | O2w—H2w2 | 0.97 |
Cu1—O5ii | 1.957 (4) | O3w—H3w1 | 0.97 |
Cu1—O7w | 1.984 (4) | O3w—H3w2 | 0.98 |
Cu1—O7wii | 1.984 (4) | O4w—H4w1 | 0.98 |
Cu1—O8w | 2.427 (4) | O4w—H4w2 | 0.97 |
Cu1—O8wii | 2.427 (4) | O5w—H5w1 | 0.97 |
O1—C1 | 1.259 (6) | O5w—H5w2 | 0.98 |
O2—C2 | 1.272 (6) | O6w—H6w1 | 0.97 |
O3—C3 | 1.264 (6) | O6w—H6w2 | 0.97 |
O4—C4 | 1.264 (6) | O7w—H7w1 | 0.98 |
O5—C5 | 1.256 (6) | O7w—H7w2 | 0.97 |
O6—C6 | 1.254 (6) | O8w—H8w1 | 0.97 |
O7—C7 | 1.251 (6) | O8w—H8w2 | 0.98 |
O8—C8 | 1.255 (6) | O9w—H9w1 | 0.99 |
C1—C2 | 1.442 (7) | O9w—H9w2 | 0.98 |
C1—C4 | 1.459 (7) | ||
O1—Ce1—O3i | 86.0 (1) | C3—O3—Ce1iii | 133.8 (3) |
O1—Ce1—O6 | 138.5 (1) | C5—O5—Cu1 | 128.9 (3) |
O1—Ce1—O1w | 62.5 (1) | C6—O6—Ce1 | 147.4 (3) |
O1—Ce1—O2w | 75.3 (1) | O1—C1—C2 | 135.1 (5) |
O1—Ce1—O3w | 81.2 (1) | O1—C1—C4 | 134.8 (5) |
O1—Ce1—O4w | 129.3 (1) | C2—C1—C4 | 90.1 (4) |
O1—Ce1—O5w | 146.5 (1) | O2—C2—C1 | 135.1 (5) |
O1—Ce1—O6w | 75.5 (1) | O2—C2—C3 | 134.6 (5) |
O3i—Ce1—O6 | 135.0 (1) | C1—C2—C3 | 90.3 (4) |
O3i—Ce1—O1w | 71.7 (1) | O3—C3—C2 | 134.7 (5) |
O3i—Ce1—O2w | 134.2 (1) | O3—C3—C4 | 135.2 (5) |
O3i—Ce1—O3w | 142.3 (1) | C2—C3—C4 | 90.1 (4) |
O3i—Ce1—O4w | 81.5 (1) | O4—C4—C3 | 133.8 (5) |
O3i—Ce1—O5w | 69.9 (1) | O4—C4—C1 | 136.8 (5) |
O3i—Ce1—O6w | 65.8 (1) | C3—C4—C1 | 89.3 (4) |
O6—Ce1—O1w | 127.1 (1) | O5—C5—C6 | 136.9 (5) |
O6—Ce1—O2w | 70.4 (1) | O5—C5—C8 | 132.7 (4) |
O6—Ce1—O3w | 68.7 (1) | C6—C5—C8 | 90.5 (4) |
O6—Ce1—O4w | 73.5 (1) | O6—C6—C5 | 134.0 (5) |
O6—Ce1—O5w | 66.9 (1) | O6—C6—C7 | 136.1 (5) |
O6—Ce1—O6w | 111.9 (1) | C5—C6—C7 | 89.9 (4) |
O1w—Ce1—O2w | 129.2 (1) | O7—C7—C8 | 135.6 (5) |
O1w—Ce1—O3w | 70.9 (1) | O7—C7—C6 | 135.1 (5) |
O1w—Ce1—O4w | 66.9 (1) | C8—C7—C6 | 89.3 (4) |
O1w—Ce1—O5w | 126.1 (1) | O8—C8—C7 | 135.4 (5) |
O1w—Ce1—O6w | 121.0 (1) | O8—C8—C5 | 134.5 (5) |
O2w—Ce1—O3w | 76.1 (1) | C7—C8—C5 | 90.1 (4) |
O2w—Ce1—O6w | 69.3 (1) | Ce1—O1w—H1w1 | 109.7 |
O2w—Ce1—O4w | 141.8 (1) | Ce1—O1w—H1w2 | 109.7 |
O2w—Ce1—O5w | 104.7 (1) | H1w1—O1w—H1w2 | 108.6 |
O3w—Ce1—O4w | 79.7 (1) | Ce1—O2w—H2w1 | 124.3 |
O3w—Ce1—O5w | 132.0 (1) | Ce1—O2w—H2w2 | 124.9 |
O3w—Ce1—O6w | 142.0 (1) | H2w1—O2w—H2w2 | 108.1 |
O4w—Ce1—O6w | 138.0 (1) | Ce1—O3w—H3w1 | 104.1 |
O4w—Ce1—O5w | 71.2 (1) | Ce1—O3w—H3w2 | 119.2 |
O5w—Ce1—O6w | 73.5 (1) | H3w1—O3w—H3w2 | 107.8 |
O5—Cu1—O5ii | 180.0 | Ce1—O4w—H4w1 | 103.5 |
O5—Cu1—O7w | 91.8 (2) | Ce1—O4w—H4w2 | 100.5 |
O5—Cu1—O7wii | 88.2 (2) | H4w1—O4w—H4w2 | 107.3 |
O5—Cu1—O8w | 92.9 (1) | Ce1—O5w—H5w1 | 105.0 |
O5—Cu1—O8wii | 87.1 (1) | Ce1—O5w—H5w2 | 104.8 |
O5ii—Cu1—O7w | 88.2 (2) | H5w1—O5w—H5w2 | 105.1 |
O5ii—Cu1—O7wii | 91.8 (2) | Ce1—O6w—H6w1 | 108.6 |
O5ii—Cu1—O8w | 87.1 (2) | Ce1—O6w—H6w2 | 112.1 |
O5ii—Cu1—O8wii | 92.9 (2) | H6w1—O6w—H6w2 | 109.1 |
O7w—Cu1—O7wii | 180.0 | Cu1—O7w—H7w1 | 109.8 |
O7w—Cu1—O8w | 95.8 (2) | Cu1—O7w—H7w2 | 109.7 |
O7w—Cu1—O8wii | 84.2 (2) | H7w1—O7w—H7w2 | 109.0 |
O7wii—Cu1—O8w | 84.2 (2) | Cu1—O8w—H8w1 | 109.5 |
O7wii—Cu1—O8wii | 95.8 (2) | Cu1—O8w—H8w2 | 117.9 |
O8w—Cu1—O8wii | 180.00 | H8w1—O8w—H8w2 | 107.3 |
C1—O1—Ce1 | 143.1 (4) | H9w1—O9w—H9w2 | 106.8 |
O3i—Ce1—O1—C1 | 100.8 (6) | O2—C2—C3—C4 | 174.3 (6) |
O3w—Ce1—O1—C1 | −114.8 (6) | C1—C2—C3—C4 | −3.9 (4) |
O6—Ce1—O1—C1 | −71.9 (7) | O3—C3—C4—O4 | 6 (1) |
O2w—Ce1—O1—C1 | −37.0 (6) | C2—C3—C4—O4 | −174.4 (6) |
O6w—Ce1—O1—C1 | 35.0 (6) | O3—C3—C4—C1 | −176.1 (6) |
O4w—Ce1—O1—C1 | 176.3 (6) | C2—C3—C4—C1 | 3.8 (4) |
O5w—Ce1—O1—C1 | 57.5 (7) | O1—C1—C4—O4 | −5 (1) |
O1w—Ce1—O1—C1 | 172.2 (7) | C2—C1—C4—O4 | 174.3 (7) |
O5ii—Cu1—O5—C5 | 0.0 (3) | O1—C1—C4—C3 | 176.8 (7) |
O7w—Cu1—O5—C5 | −55.5 (5) | C2—C1—C4—C3 | −3.8 (4) |
O7wii—Cu1—O5—C5 | 124.5 (5) | Cu1—O5—C5—C6 | 16.1 (9) |
O8wii—Cu1—O5—C5 | −139.6 (5) | Cu1—O5—C5—C8 | −161.4 (4) |
O8w—Cu1—O5—C5 | 40.4 (5) | Ce1—O6—C6—C5 | −168.4 (4) |
O3i—Ce1—O6—C6 | −119.3 (6) | Ce1—O6—C6—C7 | 15 (1) |
O1—Ce1—O6—C6 | 50.2 (7) | O5—C5—C6—O6 | 8 (1) |
O3w—Ce1—O6—C6 | 96.5 (6) | C8—C5—C6—O6 | −174.3 (6) |
O2w—Ce1—O6—C6 | 14.3 (6) | O5—C5—C6—C7 | −174.4 (6) |
O6w—Ce1—O6—C6 | −42.5 (7) | C8—C5—C6—C7 | 3.7 (4) |
O4w—Ce1—O6—C6 | −178.3 (7) | O6—C6—C7—O7 | −6 (1) |
O5w—Ce1—O6—C6 | −102.1 (6) | C5—C6—C7—O7 | 176.2 (7) |
O1w—Ce1—O6—C6 | 139.2 (6) | O6—C6—C7—C8 | 174.2 (6) |
Ce1—O1—C1—C2 | 40 (1) | C5—C6—C7—C8 | −3.7 (4) |
Ce1—O1—C1—C4 | −140.5 (5) | O7—C7—C8—O8 | 2 (1) |
O1—C1—C2—O2 | 5 (1) | C6—C7—C8—O8 | −178.6 (7) |
C4—C1—C2—O2 | −174.3 (7) | O7—C7—C8—C5 | −176.2 (7) |
O1—C1—C2—C3 | −176.8 (7) | C6—C7—C8—C5 | 3.7 (4) |
C4—C1—C2—C3 | 3.8 (4) | O5—C5—C8—O8 | −3 (1) |
Ce1iii—O3—C3—C2 | 116.7 (6) | C6—C5—C8—O8 | 178.4 (6) |
Ce1iii—O3—C3—C4 | −63.4 (9) | O5—C5—C8—C7 | 174.5 (6) |
O2—C2—C3—O3 | −6 (1) | C6—C5—C8—C7 | −3.8 (4) |
C1—C2—C3—O3 | 176.1 (6) |
Symmetry codes: (i) x−1, −y+1/2, z−1/2; (ii) −x, −y, −z; (iii) x+1, −y+1/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w2···O1 | 0.97 | 2.26 | 2.646 (5) | 103 |
O1w—H1w1···O2iv | 0.98 | 2.16 | 2.769 (5) | 119 |
O2w—H2w1···O2 | 0.98 | 1.77 | 2.734 (5) | 170 |
O2w—H2w2···O7 | 0.97 | 1.84 | 2.802 (5) | 170 |
O3w—H3w2···O4v | 0.98 | 1.90 | 2.776 (5) | 149 |
O3w—H3w1···O8w | 0.97 | 1.91 | 2.781 (5) | 149 |
O4w—H4w1···O9w | 0.98 | 1.93 | 2.696 (6) | 133 |
O4w—H4w2···O4i | 0.97 | 1.95 | 2.889 (5) | 162 |
O5w—H5w1···O8vi | 0.97 | 1.90 | 2.756 (5) | 145 |
O5w—H5w2···O9wvii | 0.98 | 2.03 | 2.943 (6) | 155 |
O6w—H6w1···O4viii | 0.97 | 1.94 | 2.706 (5) | 134 |
O6w—H6w2···O2ix | 0.97 | 1.98 | 2.923 (6) | 165 |
O7w—H7w1···O7iv | 0.98 | 2.14 | 2.909 (5) | 135 |
O7w—H7w2···O6 | 0.97 | 1.95 | 2.880 (5) | 160 |
O8w—H8w2···O8x | 0.98 | 1.80 | 2.722 (5) | 155 |
O8w—H8w1···O7xi | 0.97 | 2.01 | 2.942 (6) | 159 |
O9w—H9w1···O5ii | 0.99 | 1.98 | 2.905 (5) | 155 |
O9w—H9w2···O5wxi | 0.98 | 1.97 | 2.943 (6) | 173 |
Symmetry codes: (i) x−1, −y+1/2, z−1/2; (ii) −x, −y, −z; (iv) x−1, y, z−1; (v) x, −y+1/2, z−1/2; (vi) −x, −y, −z+1; (vii) x, y, z+1; (viii) x, −y+1/2, z+1/2; (ix) x−1, y, z; (x) −x+1, −y, −z+1; (xi) x, y, z−1. |
Experimental details
Crystal data | |
Chemical formula | [Ce(H2O)6]2[Cu(H2O)4](C4O4)4·2H2O |
Mr | 1116.23 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 298 |
a, b, c (Å) | 6.7685 (1), 32.2337 (1), 8.1730 (1) |
β (°) | 111.578 (1) |
V (Å3) | 1658.17 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 3.46 |
Crystal size (mm) | 0.32 × 0.18 × 0.04 |
Data collection | |
Diffractometer | Siemens CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.404, 0.874 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11717, 4037, 3283 |
Rint | 0.075 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.105, 1.02 |
No. of reflections | 4037 |
No. of parameters | 241 |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 1.16, −2.62 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.
Ce1—O1 | 2.456 (4) | Ce1—O6w | 2.568 (4) |
Ce1—O3i | 2.429 (4) | Cu1—O5 | 1.957 (4) |
Ce1—O6 | 2.525 (3) | Cu1—O5ii | 1.957 (4) |
Ce1—O1w | 2.635 (4) | Cu1—O7w | 1.984 (4) |
Ce1—O2w | 2.540 (4) | Cu1—O7wii | 1.984 (4) |
Ce1—O3w | 2.523 (4) | Cu1—O8w | 2.427 (4) |
Ce1—O4w | 2.582 (4) | Cu1—O8wii | 2.427 (4) |
Ce1—O5w | 2.613 (4) | ||
O1—Ce1—O3i | 86.0 (1) | O2w—Ce1—O3w | 76.1 (1) |
O1—Ce1—O6 | 138.5 (1) | O2w—Ce1—O6w | 69.3 (1) |
O1—Ce1—O1w | 62.5 (1) | O2w—Ce1—O4w | 141.8 (1) |
O1—Ce1—O2w | 75.3 (1) | O2w—Ce1—O5w | 104.7 (1) |
O1—Ce1—O3w | 81.2 (1) | O3w—Ce1—O4w | 79.7 (1) |
O1—Ce1—O4w | 129.3 (1) | O3w—Ce1—O5w | 132.0 (1) |
O1—Ce1—O5w | 146.5 (1) | O3w—Ce1—O6w | 142.0 (1) |
O1—Ce1—O6w | 75.5 (1) | O4w—Ce1—O6w | 138.0 (1) |
O3i—Ce1—O6 | 135.0 (1) | O4w—Ce1—O5w | 71.2 (1) |
O3i—Ce1—O1w | 71.7 (1) | O5w—Ce1—O6w | 73.5 (1) |
O3i—Ce1—O2w | 134.2 (1) | O5—Cu1—O5ii | 180.0 |
O3i—Ce1—O3w | 142.3 (1) | O5—Cu1—O7w | 91.8 (2) |
O3i—Ce1—O4w | 81.5 (1) | O5—Cu1—O7wii | 88.2 (2) |
O3i—Ce1—O5w | 69.9 (1) | O5—Cu1—O8w | 92.9 (1) |
O3i—Ce1—O6w | 65.8 (1) | O5—Cu1—O8wii | 87.1 (1) |
O6—Ce1—O1w | 127.1 (1) | O5ii—Cu1—O7w | 88.2 (2) |
O6—Ce1—O2w | 70.4 (1) | O5ii—Cu1—O7wii | 91.8 (2) |
O6—Ce1—O3w | 68.7 (1) | O5ii—Cu1—O8w | 87.1 (2) |
O6—Ce1—O4w | 73.5 (1) | O5ii—Cu1—O8wii | 92.9 (2) |
O6—Ce1—O5w | 66.9 (1) | O7w—Cu1—O7wii | 180.0 |
O6—Ce1—O6w | 111.9 (1) | O7w—Cu1—O8w | 95.8 (2) |
O1w—Ce1—O2w | 129.2 (1) | O7w—Cu1—O8wii | 84.2 (2) |
O1w—Ce1—O3w | 70.9 (1) | O7wii—Cu1—O8w | 84.2 (2) |
O1w—Ce1—O4w | 66.9 (1) | O7wii—Cu1—O8wii | 95.8 (2) |
O1w—Ce1—O5w | 126.1 (1) | O8w—Cu1—O8wii | 180.00 |
O1w—Ce1—O6w | 121.0 (1) |
Symmetry codes: (i) x−1, −y+1/2, z−1/2; (ii) −x, −y, −z. |
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Copper(II)–lanthanium(III) complexes having the squarate group to link the the copper and lanthanum cations are potential precursors to high-temperature superconductors as such complexes can be thermally decomposed to the oxides. Only four have been structurally characterized; the lanthanum complex exists as [La2Cu(C4O4)4(H2O)16]·2H2O, and the gadolinium and yttrium complexes as [Ln2Cu(C4O4)4(H2O)12]·2H2O (Bouayad et al., 1992). The La atom is coordinated by nine O atoms, and its geometry is assigned a monocapped square antiprism. The mixed lanthanum–samarium complex has statistically disordered La atoms; one is assigned a tricapped trigonal prismatic geometry and the other a monocapped square antiprismatic geometry (Shi et al., 1995). The assignment is, however, doubtful as the structure appears to have been refined in an unnecessarily low-symmetry space group (Ng & Hu, 2001). The lanthanum, the lanthanum–samarium and the title, (I), cerium dihydrates are isomorphous.