| Literature DB >> 22259375 |
Abstract
In the title binuclear Co(II)Entities:
Year: 2011 PMID: 22259375 PMCID: PMC3254341 DOI: 10.1107/S1600536811054602
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Co2(C12H21N2Si)2Cl2] | |
| Orthorhombic, | Mo |
| Hall symbol: -P 2ab 2ac | Cell parameters from 3365 reflections |
| θ = 2.3–26.3° | |
| µ = 1.36 mm−1 | |
| Block, green | |
| 0.20 × 0.15 × 0.10 mm |
| Bruker SMART area-detector diffractometer | 2885 independent reflections |
| Radiation source: fine-focus sealed tube | 1795 reflections with |
| graphite | |
| Detector resolution: 7.9 pixels mm-1 | θmax = 25.6°, θmin = 2.1° |
| φ and ω scan | |
| Absorption correction: multi-scan ( | |
| 16361 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-atom parameters constrained | |
| 2885 reflections | (Δ/σ)max < 0.001 |
| 154 parameters | Δρmax = 1.97 e Å−3 |
| 48 restraints | Δρmin = −0.51 e Å−3 |
| Experimental. MS (EI, 70 eV): |
| 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 | 0.55911 (8) | 0.48017 (6) | 0.43654 (6) | 0.0307 (3) | |
| Si1 | 0.37762 (17) | 0.55954 (13) | 0.36970 (13) | 0.0356 (5) | |
| Cl1 | 0.71974 (18) | 0.48946 (17) | 0.37397 (16) | 0.0617 (7) | |
| N1 | 0.4612 (5) | 0.5831 (4) | 0.4563 (4) | 0.0328 (14) | |
| N2 | 0.4195 (5) | 0.4511 (4) | 0.3528 (4) | 0.0303 (13) | |
| C1 | 0.4863 (7) | 0.6714 (5) | 0.4684 (6) | 0.0472 (14) | |
| C2 | 0.5770 (8) | 0.7089 (5) | 0.4330 (6) | 0.0534 (14) | |
| H2A | 0.6230 | 0.6770 | 0.3988 | 0.064* | |
| C3 | 0.6006 (9) | 0.7956 (6) | 0.4482 (6) | 0.0601 (15) | |
| H3A | 0.6627 | 0.8207 | 0.4250 | 0.072* | |
| C4 | 0.5322 (9) | 0.8417 (6) | 0.4969 (6) | 0.0620 (15) | |
| H4A | 0.5474 | 0.8991 | 0.5059 | 0.074* | |
| C5 | 0.4443 (8) | 0.8075 (6) | 0.5320 (7) | 0.0607 (15) | |
| H5A | 0.3997 | 0.8408 | 0.5660 | 0.073* | |
| C6 | 0.4175 (8) | 0.7207 (5) | 0.5182 (6) | 0.0536 (14) | |
| H6A | 0.3549 | 0.6971 | 0.5420 | 0.064* | |
| C7 | 0.2306 (8) | 0.5722 (7) | 0.3939 (8) | 0.079 (4) | |
| H7A | 0.1963 | 0.6064 | 0.3516 | 0.119* | |
| H7B | 0.2226 | 0.5996 | 0.4472 | 0.119* | |
| H7C | 0.1962 | 0.5171 | 0.3957 | 0.119* | |
| C8 | 0.4136 (10) | 0.6277 (6) | 0.2788 (6) | 0.073 (3) | |
| H8A | 0.3484 | 0.6541 | 0.2573 | 0.109* | |
| H8B | 0.4465 | 0.5932 | 0.2361 | 0.109* | |
| H8C | 0.4646 | 0.6710 | 0.2960 | 0.109* | |
| C9 | 0.4621 (7) | 0.4311 (5) | 0.2680 (5) | 0.0456 (18) | |
| H9A | 0.5153 | 0.4742 | 0.2523 | 0.055* | |
| H9B | 0.4019 | 0.4338 | 0.2285 | 0.055* | |
| C10 | 0.5154 (8) | 0.3447 (6) | 0.2621 (6) | 0.057 (2) | |
| H10A | 0.5407 | 0.3355 | 0.2060 | 0.085* | |
| H10B | 0.4629 | 0.3014 | 0.2765 | 0.085* | |
| H10C | 0.5765 | 0.3420 | 0.2998 | 0.085* | |
| C11 | 0.3406 (7) | 0.3856 (5) | 0.3839 (5) | 0.0468 (19) | |
| H11A | 0.3119 | 0.4042 | 0.4374 | 0.056* | |
| H11B | 0.3800 | 0.3326 | 0.3930 | 0.056* | |
| C12 | 0.2441 (8) | 0.3683 (6) | 0.3251 (6) | 0.056 (2) | |
| H12A | 0.1971 | 0.3257 | 0.3492 | 0.083* | |
| H12B | 0.2714 | 0.3483 | 0.2724 | 0.083* | |
| H12C | 0.2032 | 0.4200 | 0.3169 | 0.083* |
| Co1 | 0.0344 (5) | 0.0272 (5) | 0.0305 (6) | 0.0036 (4) | 0.0043 (4) | 0.0027 (4) |
| Si1 | 0.0450 (12) | 0.0250 (11) | 0.0369 (12) | 0.0043 (9) | −0.0108 (10) | 0.0007 (9) |
| Cl1 | 0.0470 (12) | 0.0727 (17) | 0.0655 (15) | 0.0029 (11) | 0.0246 (11) | 0.0051 (12) |
| N1 | 0.040 (3) | 0.023 (3) | 0.036 (4) | 0.005 (2) | −0.006 (3) | 0.001 (2) |
| N2 | 0.045 (3) | 0.018 (3) | 0.028 (3) | 0.000 (2) | −0.004 (3) | −0.002 (2) |
| C1 | 0.064 (3) | 0.024 (3) | 0.053 (3) | 0.001 (2) | −0.020 (3) | 0.003 (2) |
| C2 | 0.069 (3) | 0.030 (3) | 0.061 (3) | −0.004 (2) | −0.019 (3) | 0.006 (2) |
| C3 | 0.077 (3) | 0.035 (3) | 0.068 (3) | −0.006 (3) | −0.022 (3) | 0.007 (3) |
| C4 | 0.082 (3) | 0.035 (3) | 0.069 (3) | −0.001 (3) | −0.025 (3) | 0.002 (2) |
| C5 | 0.081 (3) | 0.036 (3) | 0.066 (3) | 0.007 (3) | −0.022 (3) | −0.003 (2) |
| C6 | 0.072 (3) | 0.030 (3) | 0.059 (3) | 0.005 (2) | −0.020 (3) | −0.001 (2) |
| C7 | 0.058 (6) | 0.079 (8) | 0.100 (9) | 0.027 (6) | −0.024 (6) | −0.027 (7) |
| C8 | 0.139 (10) | 0.036 (5) | 0.042 (5) | −0.014 (6) | −0.035 (6) | 0.010 (4) |
| C9 | 0.060 (5) | 0.043 (4) | 0.034 (4) | −0.003 (4) | 0.005 (3) | 0.001 (3) |
| C10 | 0.074 (5) | 0.051 (5) | 0.046 (4) | 0.004 (4) | 0.007 (4) | −0.011 (4) |
| C11 | 0.056 (4) | 0.036 (4) | 0.048 (4) | −0.008 (3) | −0.012 (4) | 0.006 (3) |
| C12 | 0.062 (4) | 0.043 (4) | 0.062 (5) | −0.014 (4) | −0.017 (4) | 0.007 (4) |
| Co1—N1i | 1.998 (6) | C5—C6 | 1.416 (12) |
| Co1—N1 | 2.031 (6) | C5—H5A | 0.9300 |
| Co1—Cl1 | 2.203 (2) | C6—H6A | 0.9300 |
| Co1—N2 | 2.214 (6) | C7—H7A | 0.9600 |
| Co1—Co1i | 2.5682 (19) | C7—H7B | 0.9600 |
| Co1—Si1 | 2.754 (2) | C7—H7C | 0.9600 |
| Si1—N1 | 1.760 (6) | C8—H8A | 0.9600 |
| Si1—N2 | 1.795 (6) | C8—H8B | 0.9600 |
| Si1—C7 | 1.843 (10) | C8—H8C | 0.9600 |
| Si1—C8 | 1.859 (9) | C9—C10 | 1.505 (12) |
| N1—C1 | 1.431 (9) | C9—H9A | 0.9700 |
| N1—Co1i | 1.998 (6) | C9—H9B | 0.9700 |
| N2—C9 | 1.487 (10) | C10—H10A | 0.9600 |
| N2—C11 | 1.492 (10) | C10—H10B | 0.9600 |
| C1—C2 | 1.375 (13) | C10—H10C | 0.9600 |
| C1—C6 | 1.391 (13) | C11—C12 | 1.531 (11) |
| C2—C3 | 1.410 (12) | C11—H11A | 0.9700 |
| C2—H2A | 0.9300 | C11—H11B | 0.9700 |
| C3—C4 | 1.351 (14) | C12—H12A | 0.9600 |
| C3—H3A | 0.9300 | C12—H12B | 0.9600 |
| C4—C5 | 1.323 (14) | C12—H12C | 0.9600 |
| C4—H4A | 0.9300 | ||
| N1i—Co1—N1 | 100.8 (2) | C5—C4—C3 | 121.9 (10) |
| N1i—Co1—Cl1 | 122.26 (18) | C5—C4—H4A | 119.1 |
| N1—Co1—Cl1 | 122.67 (19) | C3—C4—H4A | 119.1 |
| N1i—Co1—N2 | 108.9 (2) | C4—C5—C6 | 120.6 (10) |
| N1—Co1—N2 | 78.9 (2) | C4—C5—H5A | 119.7 |
| Cl1—Co1—N2 | 114.83 (18) | C6—C5—H5A | 119.7 |
| N1i—Co1—Co1i | 50.96 (17) | C1—C6—C5 | 119.0 (9) |
| N1—Co1—Co1i | 49.84 (17) | C1—C6—H6A | 120.5 |
| Cl1—Co1—Co1i | 147.37 (10) | C5—C6—H6A | 120.5 |
| N2—Co1—Co1i | 95.69 (16) | Si1—C7—H7A | 109.5 |
| N1i—Co1—Si1 | 117.33 (18) | Si1—C7—H7B | 109.5 |
| N1—Co1—Si1 | 39.67 (17) | H7A—C7—H7B | 109.5 |
| Cl1—Co1—Si1 | 120.40 (9) | Si1—C7—H7C | 109.5 |
| N2—Co1—Si1 | 40.57 (15) | H7A—C7—H7C | 109.5 |
| Co1i—Co1—Si1 | 75.44 (6) | H7B—C7—H7C | 109.5 |
| N1—Si1—N2 | 98.8 (3) | Si1—C8—H8A | 109.5 |
| N1—Si1—C7 | 111.9 (4) | Si1—C8—H8B | 109.5 |
| N2—Si1—C7 | 114.2 (4) | H8A—C8—H8B | 109.5 |
| N1—Si1—C8 | 111.2 (4) | Si1—C8—H8C | 109.5 |
| N2—Si1—C8 | 111.0 (4) | H8A—C8—H8C | 109.5 |
| C7—Si1—C8 | 109.4 (6) | H8B—C8—H8C | 109.5 |
| N1—Si1—Co1 | 47.44 (19) | N2—C9—C10 | 113.5 (7) |
| N2—Si1—Co1 | 53.33 (19) | N2—C9—H9A | 108.9 |
| C7—Si1—Co1 | 138.3 (4) | C10—C9—H9A | 108.9 |
| C8—Si1—Co1 | 112.0 (4) | N2—C9—H9B | 108.9 |
| C1—N1—Si1 | 115.7 (5) | C10—C9—H9B | 108.9 |
| C1—N1—Co1i | 112.9 (5) | H9A—C9—H9B | 107.7 |
| Si1—N1—Co1i | 120.1 (3) | C9—C10—H10A | 109.5 |
| C1—N1—Co1 | 131.6 (5) | C9—C10—H10B | 109.5 |
| Si1—N1—Co1 | 92.9 (3) | H10A—C10—H10B | 109.5 |
| Co1i—N1—Co1 | 79.2 (2) | C9—C10—H10C | 109.5 |
| C9—N2—C11 | 112.6 (6) | H10A—C10—H10C | 109.5 |
| C9—N2—Si1 | 115.9 (5) | H10B—C10—H10C | 109.5 |
| C11—N2—Si1 | 114.7 (5) | N2—C11—C12 | 114.2 (7) |
| C9—N2—Co1 | 109.2 (5) | N2—C11—H11A | 108.7 |
| C11—N2—Co1 | 115.7 (4) | C12—C11—H11A | 108.7 |
| Si1—N2—Co1 | 86.1 (2) | N2—C11—H11B | 108.7 |
| C2—C1—C6 | 118.9 (8) | C12—C11—H11B | 108.7 |
| C2—C1—N1 | 122.0 (8) | H11A—C11—H11B | 107.6 |
| C6—C1—N1 | 119.2 (8) | C11—C12—H12A | 109.5 |
| C1—C2—C3 | 120.4 (10) | C11—C12—H12B | 109.5 |
| C1—C2—H2A | 119.8 | H12A—C12—H12B | 109.5 |
| C3—C2—H2A | 119.8 | C11—C12—H12C | 109.5 |
| C4—C3—C2 | 119.3 (10) | H12A—C12—H12C | 109.5 |
| C4—C3—H3A | 120.4 | H12B—C12—H12C | 109.5 |
| C2—C3—H3A | 120.4 |