| Literature DB >> 24427006 |
Meriem Benslimane1, Yasmine Kheira Redjel1, Georges Dénès2, Hocine Merazig1.
Abstract
The title compound, [Co2(C8H7O2)4(C7H10N2)2], crystallizes as a centrosymmetric dimer containing two Co(II) atoms bridged by four bidentate phenyl-acetate ligands in syn-syn bridging modes. Each Co(II) atom is five-coordinated by four O atoms from four different carboxyl-ate ligands and the ring N atom of a 4-(di-methyl-amino)-pyridine unit, generating a distorted square-pyramidal geometry in which the four O atoms form the basal plane and the N atom occupies the axial position. In the crystal, C-H⋯O inter-actions link the dinuclear complex mol-ecules into a three-dimensional network.Entities:
Year: 2013 PMID: 24427006 PMCID: PMC3884428 DOI: 10.1107/S1600536813023258
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Co2(C8H7O2)4(C7H10N2)2] | |
| Triclinic, | |
| Hall symbol: -P 1 | Mo |
| Cell parameters from 4872 reflections | |
| θ = 2.3–25° | |
| µ = 0.86 mm−1 | |
| α = 99.766 (5)° | |
| β = 101.878 (5)° | Box, blue |
| γ = 105.335 (5)° | 0.15 × 0.1 × 0.01 mm |
| Bruker APEXII CCD diffractometer | 3645 independent reflections |
| Radiation source: fine-focus sealed tube | 3352 reflections with |
| Graphite monochromator | |
| ω and φ scans | θmax = 25.0°, θmin = 2.7° |
| Absorption correction: multi-scan ( | |
| 9238 measured reflections |
| Refinement on | 0 restraints |
| Least-squares matrix: full | H-atom parameters constrained |
| (Δ/σ)max < 0.001 | |
| Δρmax = 0.25 e Å−3 | |
| 3645 reflections | Δρmin = −0.24 e Å−3 |
| 271 parameters |
| 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 |
| Co1 | 0.56888 (3) | 0.01135 (2) | 0.114253 (18) | 0.01603 (8) | |
| O1 | 0.70384 (17) | 0.18802 (11) | 0.09742 (10) | 0.0256 (3) | |
| O3 | 0.75242 (16) | −0.06983 (12) | 0.07678 (10) | 0.0241 (3) | |
| O2 | 0.59969 (17) | 0.17191 (12) | −0.08452 (10) | 0.0248 (3) | |
| O4 | 0.64516 (17) | −0.08060 (13) | −0.10383 (10) | 0.0277 (3) | |
| N1 | 0.7414 (2) | 0.15583 (15) | 0.63408 (12) | 0.0259 (3) | |
| N2 | 0.64381 (19) | 0.06270 (13) | 0.28539 (11) | 0.0178 (3) | |
| C10 | 0.7997 (2) | 0.46694 (16) | 0.12315 (14) | 0.0192 (4) | |
| C3 | 0.7158 (2) | −0.00546 (16) | 0.34964 (14) | 0.0197 (4) | |
| H3 | 0.7415 | −0.0764 | 0.3139 | 0.024* | |
| C11 | 0.7164 (3) | 0.55861 (17) | 0.10444 (16) | 0.0256 (4) | |
| H11 | 0.6661 | 0.5599 | 0.0313 | 0.031* | |
| C1 | 0.7158 (2) | 0.12779 (17) | 0.52207 (14) | 0.0195 (4) | |
| C18 | 0.8183 (2) | −0.25048 (16) | −0.17600 (14) | 0.0181 (4) | |
| C13 | 0.7818 (3) | 0.64805 (18) | 0.30092 (16) | 0.0302 (4) | |
| H13 | 0.7766 | 0.7085 | 0.3603 | 0.036* | |
| C17 | 0.8651 (2) | −0.18185 (17) | −0.05447 (14) | 0.0205 (4) | |
| H17A | 0.9855 | −0.1236 | −0.0338 | 0.025* | |
| H17B | 0.8624 | −0.2454 | −0.0097 | 0.025* | |
| C23 | 0.9124 (2) | −0.20046 (17) | −0.24739 (15) | 0.0222 (4) | |
| H23 | 1.0052 | −0.1233 | −0.2202 | 0.027* | |
| C2 | 0.7540 (2) | 0.02208 (17) | 0.46401 (14) | 0.0216 (4) | |
| H2 | 0.8051 | −0.0289 | 0.5033 | 0.026* | |
| C19 | 0.6790 (2) | −0.36483 (17) | −0.21909 (15) | 0.0245 (4) | |
| H19 | 0.6135 | −0.399 | −0.1724 | 0.029* | |
| C9 | 0.8102 (3) | 0.37074 (16) | 0.02588 (15) | 0.0236 (4) | |
| H9A | 0.9324 | 0.3717 | 0.0358 | 0.028* | |
| H9B | 0.7754 | 0.3982 | −0.0424 | 0.028* | |
| C14 | 0.8655 (3) | 0.55707 (19) | 0.32101 (16) | 0.0311 (4) | |
| H14 | 0.9163 | 0.5563 | 0.3942 | 0.037* | |
| C4 | 0.6139 (2) | 0.16674 (17) | 0.34079 (14) | 0.0228 (4) | |
| H4 | 0.568 | 0.2179 | 0.299 | 0.027* | |
| C15 | 0.8741 (2) | 0.46726 (18) | 0.23306 (15) | 0.0267 (4) | |
| H15 | 0.9303 | 0.4063 | 0.2476 | 0.032* | |
| C5 | 0.6466 (2) | 0.20198 (17) | 0.45452 (15) | 0.0246 (4) | |
| H5 | 0.6231 | 0.2753 | 0.4876 | 0.029* | |
| C22 | 0.8696 (3) | −0.26441 (19) | −0.35918 (15) | 0.0274 (4) | |
| H22 | 0.934 | −0.23 | −0.4062 | 0.033* | |
| C16 | 0.7435 (2) | −0.10501 (16) | −0.02568 (14) | 0.0180 (4) | |
| C20 | 0.6361 (3) | −0.42857 (18) | −0.33028 (16) | 0.0291 (4) | |
| H20 | 0.5425 | −0.5053 | −0.3579 | 0.035* | |
| C12 | 0.7061 (3) | 0.64871 (18) | 0.19226 (17) | 0.0322 (5) | |
| H12 | 0.6487 | 0.7091 | 0.178 | 0.039* | |
| C8 | 0.6943 (2) | 0.23260 (16) | 0.01192 (14) | 0.0186 (4) | |
| C7 | 0.8177 (3) | 0.0810 (2) | 0.70317 (16) | 0.0328 (5) | |
| H7A | 0.8256 | 0.1152 | 0.7802 | 0.049* | |
| H7B | 0.9341 | 0.0858 | 0.6946 | 0.049* | |
| H7C | 0.7438 | −0.0076 | 0.6804 | 0.049* | |
| C21 | 0.7319 (3) | −0.37875 (19) | −0.40079 (15) | 0.0292 (4) | |
| H21 | 0.7037 | −0.4219 | −0.4756 | 0.035* | |
| C6 | 0.6940 (3) | 0.2633 (2) | 0.68950 (16) | 0.0353 (5) | |
| H6A | 0.721 | 0.2693 | 0.7686 | 0.053* | |
| H6B | 0.5694 | 0.2493 | 0.6611 | 0.053* | |
| H6C | 0.7601 | 0.3421 | 0.6754 | 0.053* |
| Co1 | 0.02007 (13) | 0.01633 (13) | 0.01213 (12) | 0.00678 (9) | 0.00475 (9) | 0.00211 (9) |
| O1 | 0.0329 (7) | 0.0188 (6) | 0.0213 (7) | 0.0030 (5) | 0.0044 (6) | 0.0066 (5) |
| O3 | 0.0262 (7) | 0.0258 (7) | 0.0218 (7) | 0.0115 (5) | 0.0093 (5) | 0.0010 (5) |
| O2 | 0.0293 (7) | 0.0213 (6) | 0.0190 (6) | 0.0020 (5) | 0.0056 (6) | 0.0022 (5) |
| O4 | 0.0278 (7) | 0.0354 (8) | 0.0261 (7) | 0.0202 (6) | 0.0074 (6) | 0.0073 (6) |
| N1 | 0.0366 (9) | 0.0275 (8) | 0.0140 (7) | 0.0111 (7) | 0.0067 (7) | 0.0044 (6) |
| N2 | 0.0212 (7) | 0.0178 (7) | 0.0146 (7) | 0.0072 (6) | 0.0048 (6) | 0.0029 (6) |
| C10 | 0.0187 (9) | 0.0152 (8) | 0.0212 (9) | 0.0001 (7) | 0.0075 (7) | 0.0034 (7) |
| C3 | 0.0234 (9) | 0.0163 (8) | 0.0209 (9) | 0.0086 (7) | 0.0065 (7) | 0.0030 (7) |
| C11 | 0.0319 (10) | 0.0201 (9) | 0.0238 (9) | 0.0060 (8) | 0.0054 (8) | 0.0080 (8) |
| C1 | 0.0196 (9) | 0.0213 (9) | 0.0160 (8) | 0.0035 (7) | 0.0054 (7) | 0.0040 (7) |
| C18 | 0.0181 (8) | 0.0187 (9) | 0.0209 (9) | 0.0111 (7) | 0.0059 (7) | 0.0041 (7) |
| C13 | 0.0418 (12) | 0.0204 (9) | 0.0283 (10) | 0.0084 (9) | 0.0156 (9) | 0.0003 (8) |
| C17 | 0.0190 (9) | 0.0212 (9) | 0.0213 (9) | 0.0081 (7) | 0.0052 (7) | 0.0023 (7) |
| C23 | 0.0182 (9) | 0.0231 (9) | 0.0252 (9) | 0.0068 (7) | 0.0047 (7) | 0.0066 (8) |
| C2 | 0.0265 (10) | 0.0217 (9) | 0.0196 (9) | 0.0109 (8) | 0.0055 (7) | 0.0085 (7) |
| C19 | 0.0248 (10) | 0.0238 (9) | 0.0256 (10) | 0.0062 (8) | 0.0090 (8) | 0.0068 (8) |
| C9 | 0.0301 (10) | 0.0185 (9) | 0.0221 (9) | 0.0041 (8) | 0.0114 (8) | 0.0047 (7) |
| C14 | 0.0390 (12) | 0.0316 (11) | 0.0200 (9) | 0.0107 (9) | 0.0046 (9) | 0.0034 (8) |
| C4 | 0.0330 (10) | 0.0216 (9) | 0.0180 (9) | 0.0151 (8) | 0.0061 (8) | 0.0057 (7) |
| C15 | 0.0289 (10) | 0.0255 (10) | 0.0270 (10) | 0.0132 (8) | 0.0043 (8) | 0.0059 (8) |
| C5 | 0.0346 (11) | 0.0213 (9) | 0.0199 (9) | 0.0144 (8) | 0.0069 (8) | 0.0016 (7) |
| C22 | 0.0283 (10) | 0.0366 (11) | 0.0224 (10) | 0.0131 (9) | 0.0097 (8) | 0.0117 (8) |
| C16 | 0.0165 (8) | 0.0139 (8) | 0.0234 (9) | 0.0029 (7) | 0.0081 (7) | 0.0030 (7) |
| C20 | 0.0277 (10) | 0.0222 (9) | 0.0285 (10) | 0.0035 (8) | 0.0000 (8) | −0.0017 (8) |
| C12 | 0.0420 (12) | 0.0205 (10) | 0.0393 (12) | 0.0154 (9) | 0.0124 (10) | 0.0098 (9) |
| C8 | 0.0189 (9) | 0.0179 (9) | 0.0208 (9) | 0.0070 (7) | 0.0089 (7) | 0.0026 (7) |
| C7 | 0.0410 (12) | 0.0410 (12) | 0.0191 (10) | 0.0146 (10) | 0.0071 (9) | 0.0124 (9) |
| C21 | 0.0347 (11) | 0.0350 (11) | 0.0169 (9) | 0.0160 (9) | 0.0022 (8) | 0.0006 (8) |
| C6 | 0.0547 (14) | 0.0327 (11) | 0.0196 (10) | 0.0140 (10) | 0.0148 (9) | 0.0022 (8) |
| Co1—O3 | 2.0224 (15) | C13—H13 | 0.93 |
| Co1—O1 | 2.0382 (14) | C17—C16 | 1.519 (2) |
| Co1—O2i | 2.0429 (15) | C17—H17A | 0.97 |
| Co1—N2 | 2.0460 (16) | C17—H17B | 0.97 |
| Co1—O4i | 2.0628 (16) | C23—C22 | 1.388 (3) |
| Co1—Co1i | 2.8020 (12) | C23—H23 | 0.93 |
| O1—C8 | 1.253 (2) | C2—H2 | 0.93 |
| O3—C16 | 1.262 (2) | C19—C20 | 1.381 (3) |
| O2—C8 | 1.256 (2) | C19—H19 | 0.93 |
| O2—Co1i | 2.0429 (15) | C9—C8 | 1.524 (2) |
| O4—C16 | 1.247 (2) | C9—H9A | 0.97 |
| O4—Co1i | 2.0628 (16) | C9—H9B | 0.97 |
| N1—C1 | 1.349 (2) | C14—C15 | 1.381 (3) |
| N1—C6 | 1.453 (2) | C14—H14 | 0.93 |
| N1—C7 | 1.454 (2) | C4—C5 | 1.366 (2) |
| N2—C3 | 1.343 (2) | C4—H4 | 0.93 |
| N2—C4 | 1.345 (2) | C15—H15 | 0.93 |
| C10—C11 | 1.383 (3) | C5—H5 | 0.93 |
| C10—C15 | 1.388 (3) | C22—C21 | 1.380 (3) |
| C10—C9 | 1.510 (2) | C22—H22 | 0.93 |
| C3—C2 | 1.369 (2) | C20—C21 | 1.384 (3) |
| C3—H3 | 0.93 | C20—H20 | 0.93 |
| C11—C12 | 1.387 (3) | C12—H12 | 0.93 |
| C11—H11 | 0.93 | C7—H7A | 0.96 |
| C1—C2 | 1.410 (2) | C7—H7B | 0.96 |
| C1—C5 | 1.411 (2) | C7—H7C | 0.96 |
| C18—C23 | 1.386 (2) | C21—H21 | 0.93 |
| C18—C19 | 1.388 (3) | C6—H6A | 0.96 |
| C18—C17 | 1.506 (2) | C6—H6B | 0.96 |
| C13—C12 | 1.380 (3) | C6—H6C | 0.96 |
| C13—C14 | 1.382 (3) | ||
| O3—Co1—O1 | 93.27 (6) | C3—C2—H2 | 120.1 |
| O3—Co1—O2i | 87.33 (6) | C1—C2—H2 | 120.1 |
| O1—Co1—O2i | 163.77 (5) | C20—C19—C18 | 120.91 (17) |
| O3—Co1—N2 | 102.92 (6) | C20—C19—H19 | 119.5 |
| O1—Co1—N2 | 94.29 (5) | C18—C19—H19 | 119.5 |
| O2i—Co1—N2 | 101.39 (5) | C10—C9—C8 | 114.21 (14) |
| O3—Co1—O4i | 163.73 (5) | C10—C9—H9A | 108.7 |
| O1—Co1—O4i | 85.64 (6) | C8—C9—H9A | 108.7 |
| O2i—Co1—O4i | 89.27 (7) | C10—C9—H9B | 108.7 |
| N2—Co1—O4i | 93.35 (5) | C8—C9—H9B | 108.7 |
| O3—Co1—Co1i | 89.34 (4) | H9A—C9—H9B | 107.6 |
| O1—Co1—Co1i | 79.04 (4) | C15—C14—C13 | 120.40 (18) |
| O2i—Co1—Co1i | 84.75 (4) | C15—C14—H14 | 119.8 |
| N2—Co1—Co1i | 166.44 (4) | C13—C14—H14 | 119.8 |
| O4i—Co1—Co1i | 74.50 (4) | N2—C4—C5 | 124.16 (16) |
| C8—O1—Co1 | 129.17 (11) | N2—C4—H4 | 117.9 |
| C16—O3—Co1 | 116.62 (11) | C5—C4—H4 | 117.9 |
| C8—O2—Co1i | 121.65 (11) | C14—C15—C10 | 120.78 (17) |
| C16—O4—Co1i | 133.30 (12) | C14—C15—H15 | 119.6 |
| C1—N1—C6 | 120.56 (16) | C10—C15—H15 | 119.6 |
| C1—N1—C7 | 121.55 (16) | C4—C5—C1 | 120.39 (16) |
| C6—N1—C7 | 117.89 (15) | C4—C5—H5 | 119.8 |
| C3—N2—C4 | 115.61 (15) | C1—C5—H5 | 119.8 |
| C3—N2—Co1 | 124.00 (11) | C21—C22—C23 | 120.28 (18) |
| C4—N2—Co1 | 120.31 (11) | C21—C22—H22 | 119.9 |
| C11—C10—C15 | 118.12 (17) | C23—C22—H22 | 119.9 |
| C11—C10—C9 | 120.35 (16) | O4—C16—O3 | 125.35 (16) |
| C15—C10—C9 | 121.52 (16) | O4—C16—C17 | 118.12 (15) |
| N2—C3—C2 | 124.67 (16) | O3—C16—C17 | 116.52 (15) |
| N2—C3—H3 | 117.7 | C19—C20—C21 | 120.23 (18) |
| C2—C3—H3 | 117.7 | C19—C20—H20 | 119.9 |
| C10—C11—C12 | 121.52 (18) | C21—C20—H20 | 119.9 |
| C10—C11—H11 | 119.2 | C13—C12—C11 | 119.52 (18) |
| C12—C11—H11 | 119.2 | C13—C12—H12 | 120.2 |
| N1—C1—C2 | 122.71 (16) | C11—C12—H12 | 120.2 |
| N1—C1—C5 | 122.05 (16) | O1—C8—O2 | 125.30 (16) |
| C2—C1—C5 | 115.23 (16) | O1—C8—C9 | 117.19 (15) |
| C23—C18—C19 | 118.53 (16) | O2—C8—C9 | 117.50 (15) |
| C23—C18—C17 | 120.81 (16) | N1—C7—H7A | 109.5 |
| C19—C18—C17 | 120.66 (16) | N1—C7—H7B | 109.5 |
| C12—C13—C14 | 119.66 (18) | H7A—C7—H7B | 109.5 |
| C12—C13—H13 | 120.2 | N1—C7—H7C | 109.5 |
| C14—C13—H13 | 120.2 | H7A—C7—H7C | 109.5 |
| C18—C17—C16 | 114.52 (14) | H7B—C7—H7C | 109.5 |
| C18—C17—H17A | 108.6 | C22—C21—C20 | 119.40 (17) |
| C16—C17—H17A | 108.6 | C22—C21—H21 | 120.3 |
| C18—C17—H17B | 108.6 | C20—C21—H21 | 120.3 |
| C16—C17—H17B | 108.6 | N1—C6—H6A | 109.5 |
| H17A—C17—H17B | 107.6 | N1—C6—H6B | 109.5 |
| C18—C23—C22 | 120.65 (17) | H6A—C6—H6B | 109.5 |
| C18—C23—H23 | 119.7 | N1—C6—H6C | 109.5 |
| C22—C23—H23 | 119.7 | H6A—C6—H6C | 109.5 |
| C3—C2—C1 | 119.85 (16) | H6B—C6—H6C | 109.5 |
| H··· | ||||
| C6—H6 | 0.96 | 2.53 | 3.337 (3) | 142 |
| C23—H23···O3iii | 0.93 | 2.58 | 3.469 (3) | 159 |
Hydrogen-bond geometry (Å, °)
|
|
| H⋯ |
|
|
|---|---|---|---|---|
| C6—H6 | 0.96 | 2.53 | 3.337 (3) | 142 |
| C23—H23⋯O3ii | 0.93 | 2.58 | 3.469 (3) | 159 |
Symmetry codes: (i) ; (ii) .