| Literature DB >> 22589823 |
Xia Yin1, Jun Fan, Jingling Xin, Shengrun Zheng, Weiguang Zhang.
Abstract
The title compound, {[Entities:
Year: 2012 PMID: 22589823 PMCID: PMC3343849 DOI: 10.1107/S1600536812011269
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Co3(C6H4NO2)2(C8H3NO6)2(H2O)2]·4H2O | |
| Triclinic, | |
| Hall symbol: -P 1 | Mo |
| Cell parameters from 3665 reflections | |
| θ = 2.0–27.9° | |
| µ = 1.57 mm−1 | |
| α = 78.74 (3)° | |
| β = 88.64 (3)° | Block, pink |
| γ = 73.68 (3)° | 0.35 × 0.28 × 0.16 mm |
| Bruker SMART APEXII CCD area-detector diffractometer | 2976 independent reflections |
| Radiation source: fine-focus sealed tube | 2667 reflections with |
| Graphite monochromator | |
| φ and ω scan | θmax = 25.3°, θmin = 2.0° |
| Absorption correction: multi-scan ( | |
| 4357 measured reflections |
| Refinement on | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| Hydrogen site location: inferred from neighbouring sites | |
| H atoms treated by a mixture of independent and constrained refinement | |
| 2976 reflections | (Δ/σ)max = 0.001 |
| 271 parameters | Δρmax = 0.40 e Å−3 |
| 10 restraints | Δρmin = −0.40 e Å−3 |
| Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
| Refinement. Refinement of |
| Occ. (<1) | |||||
| C1 | −0.1582 (2) | 0.6886 (2) | 0.7129 (2) | 0.0192 (5) | |
| C2 | −0.1920 (3) | 0.8433 (2) | 0.6267 (2) | 0.0193 (5) | |
| C3 | −0.2761 (3) | 0.8738 (2) | 0.5103 (2) | 0.0215 (5) | |
| H3 | −0.3109 | 0.7991 | 0.4846 | 0.026* | |
| C4 | −0.3067 (3) | 1.0182 (3) | 0.4336 (2) | 0.0226 (5) | |
| C5 | −0.2494 (3) | 1.1290 (3) | 0.4646 (2) | 0.0241 (5) | |
| H5 | −0.2671 | 1.2232 | 0.4086 | 0.029* | |
| C6 | −0.1647 (3) | 1.0974 (2) | 0.5811 (2) | 0.0194 (5) | |
| C7 | −0.1408 (3) | 0.9561 (2) | 0.6638 (2) | 0.0212 (5) | |
| H7 | −0.0902 | 0.9370 | 0.7445 | 0.025* | |
| C9 | 0.2058 (2) | 0.3927 (2) | 0.7504 (2) | 0.0201 (5) | |
| C10 | 0.3646 (2) | 0.3974 (2) | 0.7775 (2) | 0.0201 (5) | |
| C11 | 0.4307 (3) | 0.3616 (3) | 0.9022 (2) | 0.0302 (6) | |
| H11 | 0.3769 | 0.3339 | 0.9753 | 0.036* | |
| C12 | 0.5780 (3) | 0.3674 (3) | 0.9166 (2) | 0.0291 (5) | |
| H12 | 0.6227 | 0.3388 | 1.0005 | 0.035* | |
| C13 | 0.5920 (3) | 0.4501 (3) | 0.6972 (2) | 0.0320 (6) | |
| H13 | 0.6454 | 0.4836 | 0.6259 | 0.038* | |
| C14 | 0.4490 (3) | 0.4422 (3) | 0.6743 (2) | 0.0313 (6) | |
| H14 | 0.4085 | 0.4672 | 0.5889 | 0.038* | |
| C8 | −0.1022 (2) | 1.2189 (2) | 0.6151 (2) | 0.0202 (5) | |
| Co1 | 0.0000 | 0.5000 | 0.5000 | 0.01527 (11) | |
| Co2 | −0.10352 (3) | 0.39808 (3) | 0.82492 (3) | 0.01738 (10) | |
| N2 | 0.6596 (2) | 0.4120 (2) | 0.81683 (18) | 0.0218 (4) | |
| N1 | −0.4063 (2) | 1.0548 (2) | 0.3153 (2) | 0.0297 (5) | |
| O2 | −0.1492 (2) | 0.67118 (19) | 0.83422 (16) | 0.0285 (4) | |
| O1 | −0.14157 (17) | 0.57462 (16) | 0.65704 (15) | 0.0192 (3) | |
| O6 | −0.4433 (3) | 0.9517 (2) | 0.2817 (2) | 0.0474 (5) | |
| O5 | −0.4506 (3) | 1.1871 (2) | 0.2580 (2) | 0.0484 (5) | |
| O7 | 0.11919 (18) | 0.3888 (2) | 0.84536 (16) | 0.0285 (4) | |
| O3 | −0.07060 (19) | 1.21068 (17) | 0.73447 (16) | 0.0247 (4) | |
| O4 | −0.08995 (18) | 1.31976 (17) | 0.52098 (16) | 0.0250 (4) | |
| O8 | 0.17412 (17) | 0.39430 (18) | 0.63366 (15) | 0.0231 (3) | |
| O1W | 0.8479 (2) | 0.0405 (2) | 0.1145 (2) | 0.0498 (5) | |
| H1W | 0.9262 | −0.0299 | 0.1429 | 0.075* | |
| H2W | 0.8017 | 0.0109 | 0.0599 | 0.075* | |
| O3W | −0.0897 (2) | 0.2994 (2) | 1.01711 (16) | 0.0356 (4) | |
| H5W | −0.0190 | 0.3181 | 1.0515 | 0.053* | |
| H6W | −0.1021 | 0.2183 | 1.0577 | 0.053* | |
| O2W | 0.3255 (3) | 0.0491 (3) | 0.0522 (3) | 0.0676 (7) | |
| H4WA | 0.271 (8) | 0.114 (6) | 0.094 (7) | 0.101* | 0.50 |
| H3WA | 0.386 (8) | −0.021 (7) | 0.103 (6) | 0.101* | 0.50 |
| H3WB | 0.415 (3) | −0.006 (6) | 0.038 (6) | 0.101* | 0.50 |
| H4WB | 0.344 (5) | 0.096 (5) | 0.114 (5) | 0.101* | 0.50 |
| C1 | 0.0180 (11) | 0.0210 (11) | 0.0200 (12) | −0.0090 (9) | −0.0018 (9) | −0.0017 (9) |
| C2 | 0.0203 (11) | 0.0170 (11) | 0.0211 (12) | −0.0057 (9) | 0.0012 (9) | −0.0046 (9) |
| C3 | 0.0245 (12) | 0.0198 (11) | 0.0226 (12) | −0.0085 (9) | 0.0000 (9) | −0.0067 (9) |
| C4 | 0.0246 (12) | 0.0229 (12) | 0.0205 (12) | −0.0059 (9) | −0.0043 (9) | −0.0050 (9) |
| C5 | 0.0285 (13) | 0.0181 (11) | 0.0244 (13) | −0.0068 (9) | 0.0002 (10) | −0.0009 (9) |
| C6 | 0.0226 (11) | 0.0168 (10) | 0.0212 (11) | −0.0087 (9) | 0.0018 (9) | −0.0049 (9) |
| C7 | 0.0244 (12) | 0.0227 (11) | 0.0185 (11) | −0.0095 (9) | −0.0006 (9) | −0.0044 (9) |
| C9 | 0.0164 (11) | 0.0186 (11) | 0.0247 (13) | −0.0058 (9) | −0.0022 (9) | −0.0012 (9) |
| C10 | 0.0165 (11) | 0.0222 (11) | 0.0224 (12) | −0.0059 (9) | −0.0030 (9) | −0.0047 (9) |
| C11 | 0.0256 (13) | 0.0474 (15) | 0.0193 (12) | −0.0183 (11) | −0.0009 (10) | 0.0010 (11) |
| C12 | 0.0247 (13) | 0.0447 (15) | 0.0191 (12) | −0.0142 (11) | −0.0049 (10) | −0.0017 (11) |
| C13 | 0.0258 (13) | 0.0518 (16) | 0.0201 (13) | −0.0196 (12) | 0.0000 (10) | 0.0016 (11) |
| C14 | 0.0237 (13) | 0.0541 (17) | 0.0186 (13) | −0.0191 (12) | −0.0043 (10) | −0.0003 (11) |
| C8 | 0.0164 (11) | 0.0173 (11) | 0.0274 (13) | −0.0048 (9) | −0.0008 (9) | −0.0053 (9) |
| Co1 | 0.0164 (2) | 0.0163 (2) | 0.0144 (2) | −0.00812 (16) | −0.00199 (16) | −0.00068 (16) |
| Co2 | 0.01635 (17) | 0.02053 (17) | 0.01603 (17) | −0.00834 (12) | −0.00217 (11) | −0.00047 (12) |
| N2 | 0.0185 (10) | 0.0277 (10) | 0.0205 (10) | −0.0088 (8) | −0.0011 (8) | −0.0042 (8) |
| N1 | 0.0334 (12) | 0.0289 (11) | 0.0256 (11) | −0.0078 (9) | −0.0075 (9) | −0.0031 (9) |
| O2 | 0.0386 (10) | 0.0315 (9) | 0.0176 (9) | −0.0147 (8) | −0.0028 (7) | −0.0024 (7) |
| O1 | 0.0226 (8) | 0.0158 (7) | 0.0209 (8) | −0.0086 (6) | 0.0011 (6) | −0.0028 (6) |
| O6 | 0.0637 (14) | 0.0393 (11) | 0.0429 (12) | −0.0196 (10) | −0.0279 (10) | −0.0057 (9) |
| O5 | 0.0636 (14) | 0.0314 (11) | 0.0423 (12) | −0.0081 (10) | −0.0262 (10) | 0.0072 (9) |
| O7 | 0.0183 (8) | 0.0470 (10) | 0.0226 (9) | −0.0141 (7) | −0.0003 (7) | −0.0050 (8) |
| O3 | 0.0308 (9) | 0.0209 (8) | 0.0242 (9) | −0.0095 (7) | −0.0051 (7) | −0.0048 (7) |
| O4 | 0.0319 (9) | 0.0219 (8) | 0.0254 (9) | −0.0163 (7) | −0.0005 (7) | −0.0013 (7) |
| O8 | 0.0211 (8) | 0.0282 (8) | 0.0200 (9) | −0.0062 (7) | −0.0051 (6) | −0.0051 (7) |
| O1W | 0.0499 (13) | 0.0354 (11) | 0.0605 (14) | −0.0130 (10) | −0.0197 (11) | 0.0029 (10) |
| O3W | 0.0370 (11) | 0.0510 (11) | 0.0227 (9) | −0.0284 (9) | −0.0097 (8) | 0.0079 (8) |
| O2W | 0.0697 (18) | 0.0779 (19) | 0.0591 (16) | −0.0224 (14) | −0.0130 (14) | −0.0186 (14) |
| C1—O2 | 1.241 (3) | C8—O4 | 1.246 (3) |
| C1—O1 | 1.281 (3) | C8—O3 | 1.263 (3) |
| C1—C2 | 1.499 (3) | Co1—O8 | 2.0363 (17) |
| C2—C3 | 1.388 (3) | Co1—O8i | 2.0363 (17) |
| C2—C7 | 1.389 (3) | Co1—O4ii | 2.0506 (15) |
| C3—C4 | 1.384 (3) | Co1—O4iii | 2.0506 (15) |
| C3—H3 | 0.9300 | Co1—O1 | 2.1623 (16) |
| C4—C5 | 1.379 (3) | Co1—O1i | 2.1623 (16) |
| C4—N1 | 1.477 (3) | Co2—O3W | 2.0205 (18) |
| C5—C6 | 1.391 (3) | Co2—O7 | 2.0383 (16) |
| C5—H5 | 0.9300 | Co2—O3ii | 2.0927 (16) |
| C6—C7 | 1.391 (3) | Co2—O1 | 2.1146 (17) |
| C6—C8 | 1.511 (3) | Co2—N2iv | 2.1468 (19) |
| C7—H7 | 0.9300 | N2—Co2v | 2.1468 (19) |
| C9—O8 | 1.250 (3) | N1—O6 | 1.220 (3) |
| C9—O7 | 1.254 (3) | N1—O5 | 1.222 (3) |
| C9—C10 | 1.507 (3) | O3—Co2vi | 2.0927 (16) |
| C10—C14 | 1.376 (3) | O4—Co1vi | 2.0506 (15) |
| C10—C11 | 1.384 (3) | O1W—H1W | 0.8406 |
| C11—C12 | 1.383 (3) | O1W—H2W | 0.8463 |
| C11—H11 | 0.9300 | O3W—H5W | 0.8243 |
| C12—N2 | 1.334 (3) | O3W—H6W | 0.8285 |
| C12—H12 | 0.9300 | O2W—H4WA | 0.854 (19) |
| C13—N2 | 1.341 (3) | O2W—H3WA | 0.83 (2) |
| C13—C14 | 1.366 (3) | O2W—H3WB | 0.868 (19) |
| C13—H13 | 0.9300 | O2W—H4WB | 0.886 (18) |
| C14—H14 | 0.9300 | ||
| O2—C1—O1 | 120.9 (2) | O8—Co1—O4iii | 84.51 (7) |
| O2—C1—C2 | 121.4 (2) | O8i—Co1—O4iii | 95.49 (7) |
| O1—C1—C2 | 117.69 (19) | O4ii—Co1—O4iii | 180.0 |
| C3—C2—C7 | 120.2 (2) | O8—Co1—O1 | 89.18 (6) |
| C3—C2—C1 | 119.64 (19) | O8i—Co1—O1 | 90.82 (6) |
| C7—C2—C1 | 120.2 (2) | O4ii—Co1—O1 | 87.91 (6) |
| C4—C3—C2 | 118.2 (2) | O4iii—Co1—O1 | 92.09 (6) |
| C4—C3—H3 | 120.9 | O8—Co1—O1i | 90.82 (6) |
| C2—C3—H3 | 120.9 | O8i—Co1—O1i | 89.18 (6) |
| C5—C4—C3 | 122.5 (2) | O4ii—Co1—O1i | 92.09 (6) |
| C5—C4—N1 | 119.0 (2) | O4iii—Co1—O1i | 87.91 (6) |
| C3—C4—N1 | 118.4 (2) | O1—Co1—O1i | 180.0 |
| C4—C5—C6 | 118.8 (2) | O3W—Co2—O7 | 86.46 (7) |
| C4—C5—H5 | 120.6 | O3W—Co2—O3ii | 101.78 (7) |
| C6—C5—H5 | 120.6 | O7—Co2—O3ii | 97.35 (7) |
| C5—C6—C7 | 119.6 (2) | O3W—Co2—O1 | 158.16 (7) |
| C5—C6—C8 | 118.8 (2) | O7—Co2—O1 | 93.45 (7) |
| C7—C6—C8 | 121.6 (2) | O3ii—Co2—O1 | 99.89 (6) |
| C2—C7—C6 | 120.5 (2) | O3W—Co2—N2iv | 90.42 (8) |
| C2—C7—H7 | 119.8 | O7—Co2—N2iv | 175.95 (7) |
| C6—C7—H7 | 119.8 | O3ii—Co2—N2iv | 85.80 (7) |
| O8—C9—O7 | 126.8 (2) | O1—Co2—N2iv | 88.50 (7) |
| O8—C9—C10 | 115.7 (2) | C12—N2—C13 | 116.3 (2) |
| O7—C9—C10 | 117.6 (2) | C12—N2—Co2v | 126.40 (16) |
| C14—C10—C11 | 117.4 (2) | C13—N2—Co2v | 116.62 (15) |
| C14—C10—C9 | 119.2 (2) | O6—N1—O5 | 123.4 (2) |
| C11—C10—C9 | 123.4 (2) | O6—N1—C4 | 118.2 (2) |
| C12—C11—C10 | 119.0 (2) | O5—N1—C4 | 118.4 (2) |
| C12—C11—H11 | 120.5 | C1—O1—Co2 | 99.61 (13) |
| C10—C11—H11 | 120.5 | C1—O1—Co1 | 132.30 (13) |
| N2—C12—C11 | 123.7 (2) | Co2—O1—Co1 | 110.24 (7) |
| N2—C12—H12 | 118.2 | C9—O7—Co2 | 122.97 (15) |
| C11—C12—H12 | 118.2 | C8—O3—Co2vi | 124.57 (14) |
| N2—C13—C14 | 123.5 (2) | C8—O4—Co1vi | 134.35 (15) |
| N2—C13—H13 | 118.3 | C9—O8—Co1 | 138.09 (15) |
| C14—C13—H13 | 118.3 | H1W—O1W—H2W | 108.3 |
| C13—C14—C10 | 120.1 (2) | Co2—O3W—H5W | 107.7 |
| C13—C14—H14 | 120.0 | Co2—O3W—H6W | 133.6 |
| C10—C14—H14 | 120.0 | H5W—O3W—H6W | 109.9 |
| O4—C8—O3 | 126.6 (2) | H4WA—O2W—H3WA | 111 (4) |
| O4—C8—C6 | 115.6 (2) | H4WA—O2W—H3WB | 149 (7) |
| O3—C8—C6 | 117.70 (19) | H3WA—O2W—H3WB | 51 (7) |
| O8—Co1—O8i | 180.000 (1) | H4WA—O2W—H4WB | 46 (6) |
| O8—Co1—O4ii | 95.49 (7) | H3WA—O2W—H4WB | 77 (6) |
| O8i—Co1—O4ii | 84.51 (7) | H3WB—O2W—H4WB | 103 (3) |
| O2—C1—C2—C3 | −146.5 (2) | C3—C4—N1—O5 | 169.9 (2) |
| O1—C1—C2—C3 | 32.3 (3) | O2—C1—O1—Co2 | 0.1 (2) |
| O2—C1—C2—C7 | 32.7 (3) | C2—C1—O1—Co2 | −178.70 (16) |
| O1—C1—C2—C7 | −148.5 (2) | O2—C1—O1—Co1 | −128.83 (19) |
| C7—C2—C3—C4 | 0.0 (3) | C2—C1—O1—Co1 | 52.4 (3) |
| C1—C2—C3—C4 | 179.3 (2) | O3W—Co2—O1—C1 | 8.5 (2) |
| C2—C3—C4—C5 | 4.0 (3) | O7—Co2—O1—C1 | −80.54 (13) |
| C2—C3—C4—N1 | −175.2 (2) | O3ii—Co2—O1—C1 | −178.62 (13) |
| C3—C4—C5—C6 | −3.7 (4) | N2iv—Co2—O1—C1 | 95.91 (13) |
| N1—C4—C5—C6 | 175.4 (2) | O3W—Co2—O1—Co1 | 150.72 (15) |
| C4—C5—C6—C7 | −0.5 (3) | O7—Co2—O1—Co1 | 61.64 (8) |
| C4—C5—C6—C8 | −179.9 (2) | O3ii—Co2—O1—Co1 | −36.44 (8) |
| C3—C2—C7—C6 | −4.1 (3) | N2iv—Co2—O1—Co1 | −121.91 (8) |
| C1—C2—C7—C6 | 176.6 (2) | O8—Co1—O1—C1 | 84.14 (19) |
| C5—C6—C7—C2 | 4.4 (3) | O8i—Co1—O1—C1 | −95.86 (19) |
| C8—C6—C7—C2 | −176.2 (2) | O4ii—Co1—O1—C1 | 179.66 (19) |
| O8—C9—C10—C14 | 16.8 (3) | O4iii—Co1—O1—C1 | −0.34 (19) |
| O7—C9—C10—C14 | −162.7 (2) | O8—Co1—O1—Co2 | −41.04 (7) |
| O8—C9—C10—C11 | −164.6 (2) | O8i—Co1—O1—Co2 | 138.96 (7) |
| O7—C9—C10—C11 | 16.0 (3) | O4ii—Co1—O1—Co2 | 54.48 (8) |
| C14—C10—C11—C12 | −2.2 (4) | O4iii—Co1—O1—Co2 | −125.52 (8) |
| C9—C10—C11—C12 | 179.2 (2) | O8—C9—O7—Co2 | −4.1 (3) |
| C10—C11—C12—N2 | 2.8 (4) | C10—C9—O7—Co2 | 175.29 (14) |
| N2—C13—C14—C10 | 1.9 (4) | O3W—Co2—O7—C9 | 157.95 (19) |
| C11—C10—C14—C13 | 0.0 (4) | O3ii—Co2—O7—C9 | 56.52 (18) |
| C9—C10—C14—C13 | 178.7 (2) | O1—Co2—O7—C9 | −43.92 (18) |
| C5—C6—C8—O4 | −21.3 (3) | O4—C8—O3—Co2vi | 35.3 (3) |
| C7—C6—C8—O4 | 159.2 (2) | C6—C8—O3—Co2vi | −143.13 (16) |
| C5—C6—C8—O3 | 157.3 (2) | O3—C8—O4—Co1vi | 7.4 (4) |
| C7—C6—C8—O3 | −22.2 (3) | C6—C8—O4—Co1vi | −174.15 (14) |
| C11—C12—N2—C13 | −1.0 (4) | O7—C9—O8—Co1 | 43.6 (4) |
| C11—C12—N2—Co2v | −171.6 (2) | C10—C9—O8—Co1 | −135.76 (18) |
| C14—C13—N2—C12 | −1.3 (4) | O4ii—Co1—O8—C9 | −101.0 (2) |
| C14—C13—N2—Co2v | 170.1 (2) | O4iii—Co1—O8—C9 | 79.0 (2) |
| C5—C4—N1—O6 | 172.6 (2) | O1—Co1—O8—C9 | −13.2 (2) |
| C3—C4—N1—O6 | −8.3 (3) | O1i—Co1—O8—C9 | 166.8 (2) |
| C5—C4—N1—O5 | −9.3 (3) |
| H··· | ||||
| O1 | 0.84 | 2.05 | 2.861 (3) | 160 |
| O1 | 0.85 | 1.93 | 2.773 (3) | 173 |
| O3 | 0.82 | 2.01 | 2.820 (2) | 168 |
| O3 | 0.83 | 1.83 | 2.648 (3) | 167 |
| O2 | 0.85 (2) | 2.27 (2) | 3.098 (4) | 165 (8) |
| O2 | 0.83 (2) | 2.38 (6) | 3.055 (3) | 138 (8) |
| O2 | 0.87 (2) | 2.49 (3) | 3.297 (6) | 154 (6) |
| O2 | 0.89 (5) | 2.54 (5) | 3.055 (4) | 118 (3) |
| O2 | 0.89 (5) | 2.54 (5) | 3.098 (3) | 121 (4) |
Hydrogen-bond geometry (Å, °)
| H⋯ | ||||
|---|---|---|---|---|
| O1 | 0.84 | 2.05 | 2.861 (3) | 160 |
| O1 | 0.85 | 1.93 | 2.773 (3) | 173 |
| O3 | 0.82 | 2.01 | 2.820 (2) | 168 |
| O3 | 0.83 | 1.83 | 2.648 (3) | 167 |
| O2 | 0.85 (2) | 2.27 (2) | 3.098 (4) | 165 (8) |
| O2 | 0.83 (2) | 2.38 (6) | 3.055 (3) | 138 (8) |
| O2 | 0.87 (2) | 2.49 (3) | 3.297 (6) | 154 (6) |
| O2 | 0.89 (5) | 2.54 (5) | 3.055 (4) | 118 (3) |
| O2 | 0.89 (5) | 2.54 (5) | 3.098 (3) | 121 (4) |
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .