Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801015446/cv6061sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801015446/cv6061Isup2.hkl |
CCDC reference: 175344
Ethylenediamine, 4-acetyl pyridine and cobalt(II) thiocyanate were obtained from Aldrich. The N,N'-bis(4-acetylpyrilidene)ethylenediamine component was prepared in the following manner: 1 ml (15 mmol) of distilled ethylenediamine and 3.32 ml (30 mmol) of freshly distilled 4-acetylpyridine) were refluxed in 50 ml of anhydrous methanol for 6 h. On evaporation of the solvent, a yellow semi-solid was obtained, which on recrystallization from n-hexane gave colorless needles of N,N'-bis(4-acetylpyrilidene)ethylenediamine. Yield: 2.30 g (58%); m.p. 446–448 K. Analysis found (calculated): C 72.29 (72.14), H 6.92 (6.82), N 20.97% (21.04%). EI—MS: m/z 267.1 (MH+, 90%), 237.1 (MH+ - 2CH3, 12%). 1H NMR (200 MHz, CDCl3, TMS): δ 8.64 (d, J = 4 Hz, 4H), 7.60 (d, J = 4 Hz, 4H), 3.94 (s, methylene, 4H), 2.28 (s, methyl, 6H). 13C NMR (200 MHz, CDCl3, TMS): δ 164.54, 150.14, 147.74, 121.19, 53.35, 15.66. 0.13 g (0.5 mmol) of the latter product was dissolved in 30 ml me thanol, and added 10 ml water solution of 0.09 g (0.5 mmol) cobalt(II) thiocyanate with constant stirring. The resulting red–yellow solution was kept in the refrigerator for three days until yellow crystals of the title compound separated out. They were filtered off and dried in air. Yield: 0.15 g (45%).
Data collection: COLLECT (Nonius B.V., 1999); cell refinement: DENZO (Otwinowski, 1985); data reduction: DENZO (Otwinowski, 1985); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXL97.
[Co(NCS)2(C7H7NO)4] | Dx = 1.387 Mg m−3 |
Mr = 659.63 | Melting point: 173-175 °C K |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
a = 11.9180 (2) Å | Cell parameters from 4541 reflections |
b = 15.9700 (2) Å | θ = 2.8–27.9° |
c = 33.1930 (6) Å | µ = 0.72 mm−1 |
V = 6317.64 (17) Å3 | T = 110 K |
Z = 8 | Prism, yellow-red |
F(000) = 2728 | 0.25 × 0.20 × 0.10 mm |
Nonius KappaCCD diffractometer | 7506 independent reflections |
Radiation source: fine-focus sealed tube | 4541 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.063 |
Detector resolution: 56 microns pixels mm-1 | θmax = 27.9°, θmin = 2.8° |
1.0° ϕ scans | h = 0→15 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = 0→20 |
Tmin = 0.841, Tmax = 0.932 | l = 0→43 |
14852 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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.115 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0525P)2 + 0.1175P] where P = (Fo2 + 2Fc2)/3 |
7506 reflections | (Δ/σ)max = 0.010 |
392 parameters | Δρmax = 0.38 e Å−3 |
0 restraints | Δρmin = −0.39 e Å−3 |
[Co(NCS)2(C7H7NO)4] | V = 6317.64 (17) Å3 |
Mr = 659.63 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 11.9180 (2) Å | µ = 0.72 mm−1 |
b = 15.9700 (2) Å | T = 110 K |
c = 33.1930 (6) Å | 0.25 × 0.20 × 0.10 mm |
Nonius KappaCCD diffractometer | 7506 independent reflections |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | 4541 reflections with I > 2σ(I) |
Tmin = 0.841, Tmax = 0.932 | Rint = 0.063 |
14852 measured reflections |
R[F2 > 2σ(F2)] = 0.046 | 0 restraints |
wR(F2) = 0.115 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.38 e Å−3 |
7506 reflections | Δρmin = −0.39 e Å−3 |
392 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 F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.44893 (3) | 0.061308 (19) | 0.130607 (10) | 0.02267 (11) | |
N2 | 0.49857 (18) | −0.05290 (12) | 0.10731 (7) | 0.0289 (5) | |
C3 | 0.5356 (2) | −0.11995 (16) | 0.10372 (7) | 0.0263 (6) | |
S4 | 0.59144 (7) | −0.21263 (4) | 0.09935 (2) | 0.0429 (2) | |
N5 | 0.40083 (17) | 0.17406 (12) | 0.15618 (6) | 0.0263 (5) | |
C6 | 0.3562 (2) | 0.22487 (15) | 0.17532 (8) | 0.0242 (6) | |
S7 | 0.29491 (6) | 0.29716 (5) | 0.20202 (2) | 0.0409 (2) | |
N8 | 0.27963 (17) | 0.04679 (11) | 0.10652 (6) | 0.0239 (5) | |
C9 | 0.2154 (2) | 0.11319 (15) | 0.09877 (7) | 0.0278 (6) | |
H9 | 0.2428 | 0.1670 | 0.1060 | 0.033* | |
C10 | 0.1111 (2) | 0.10797 (15) | 0.08075 (8) | 0.0272 (6) | |
H10 | 0.0687 | 0.1572 | 0.0757 | 0.033* | |
C11 | 0.0692 (2) | 0.03039 (15) | 0.07009 (8) | 0.0258 (6) | |
C12 | 0.1343 (2) | −0.03966 (15) | 0.07908 (8) | 0.0315 (6) | |
H12 | 0.1079 | −0.0942 | 0.0728 | 0.038* | |
C13 | 0.2376 (2) | −0.02884 (15) | 0.09729 (8) | 0.0310 (6) | |
H13 | 0.2809 | −0.0771 | 0.1036 | 0.037* | |
C14 | −0.0407 (2) | 0.01980 (17) | 0.04860 (8) | 0.0329 (6) | |
C15 | −0.0980 (2) | 0.09532 (17) | 0.03205 (9) | 0.0419 (8) | |
H15A | −0.1655 | 0.0782 | 0.0173 | 0.063* | |
H15B | −0.0470 | 0.1248 | 0.0137 | 0.063* | |
H15C | −0.1191 | 0.1327 | 0.0542 | 0.063* | |
O16 | −0.08074 (17) | −0.04936 (12) | 0.04459 (7) | 0.0525 (6) | |
N17 | 0.62281 (17) | 0.08328 (12) | 0.15254 (6) | 0.0241 (5) | |
C18 | 0.6445 (2) | 0.13397 (15) | 0.18366 (8) | 0.0280 (6) | |
H18 | 0.5829 | 0.1566 | 0.1982 | 0.034* | |
C19 | 0.7526 (2) | 0.15539 (15) | 0.19589 (8) | 0.0286 (6) | |
H19 | 0.7642 | 0.1930 | 0.2177 | 0.034* | |
C20 | 0.8428 (2) | 0.12062 (15) | 0.17556 (8) | 0.0266 (6) | |
C21 | 0.8209 (2) | 0.06782 (15) | 0.14359 (8) | 0.0283 (6) | |
H21 | 0.8811 | 0.0431 | 0.1291 | 0.034* | |
C22 | 0.7112 (2) | 0.05100 (15) | 0.13268 (8) | 0.0272 (6) | |
H22 | 0.6978 | 0.0153 | 0.1103 | 0.033* | |
C23 | 0.9632 (2) | 0.13682 (17) | 0.18784 (8) | 0.0331 (7) | |
C24 | 0.9890 (2) | 0.21469 (19) | 0.21046 (10) | 0.0475 (8) | |
H24A | 1.0705 | 0.2205 | 0.2133 | 0.071* | |
H24B | 0.9545 | 0.2119 | 0.2372 | 0.071* | |
H24C | 0.9591 | 0.2630 | 0.1958 | 0.071* | |
O25 | 1.03449 (16) | 0.08539 (13) | 0.17840 (6) | 0.0471 (5) | |
N26 | 0.51032 (17) | 0.12610 (12) | 0.07626 (6) | 0.0253 (5) | |
C27 | 0.5373 (2) | 0.08720 (16) | 0.04180 (8) | 0.0295 (6) | |
H27 | 0.5118 | 0.0314 | 0.0379 | 0.035* | |
C28 | 0.6000 (2) | 0.12373 (16) | 0.01176 (8) | 0.0311 (6) | |
H28 | 0.6154 | 0.0938 | −0.0123 | 0.037* | |
C29 | 0.6405 (2) | 0.20443 (15) | 0.01680 (8) | 0.0273 (6) | |
C30 | 0.6113 (2) | 0.24601 (16) | 0.05182 (8) | 0.0329 (7) | |
H30 | 0.6363 | 0.3017 | 0.0564 | 0.039* | |
C31 | 0.5456 (2) | 0.20573 (15) | 0.08011 (8) | 0.0295 (6) | |
H31 | 0.5242 | 0.2359 | 0.1035 | 0.035* | |
C32 | 0.7193 (2) | 0.24147 (16) | −0.01386 (9) | 0.0341 (7) | |
C33 | 0.7771 (2) | 0.32178 (17) | −0.00378 (9) | 0.0404 (7) | |
H33A | 0.8252 | 0.3385 | −0.0263 | 0.061* | |
H33B | 0.8230 | 0.3141 | 0.0204 | 0.061* | |
H33C | 0.7209 | 0.3654 | 0.0012 | 0.061* | |
O34 | 0.73596 (18) | 0.20415 (11) | −0.04543 (6) | 0.0469 (6) | |
N35 | 0.40096 (17) | 0.00254 (11) | 0.18639 (6) | 0.0239 (5) | |
C36 | 0.3011 (2) | 0.01651 (15) | 0.20425 (8) | 0.0251 (6) | |
H36 | 0.2482 | 0.0515 | 0.1911 | 0.030* | |
C37 | 0.2731 (2) | −0.01791 (14) | 0.24070 (7) | 0.0231 (6) | |
H37 | 0.2008 | −0.0085 | 0.2518 | 0.028* | |
C38 | 0.3510 (2) | −0.06675 (14) | 0.26139 (7) | 0.0232 (6) | |
C39 | 0.4547 (2) | −0.07981 (14) | 0.24344 (8) | 0.0247 (6) | |
H39 | 0.5108 | −0.1115 | 0.2569 | 0.030* | |
C40 | 0.4753 (2) | −0.04655 (14) | 0.20614 (8) | 0.0262 (6) | |
H40 | 0.5451 | −0.0585 | 0.1936 | 0.031* | |
C41 | 0.3187 (2) | −0.10567 (15) | 0.30053 (8) | 0.0297 (6) | |
C42 | 0.4093 (2) | −0.13244 (18) | 0.32917 (9) | 0.0410 (7) | |
H42A | 0.3758 | −0.1470 | 0.3552 | 0.061* | |
H42B | 0.4628 | −0.0865 | 0.3328 | 0.061* | |
H42C | 0.4484 | −0.1813 | 0.3182 | 0.061* | |
O43 | 0.21969 (16) | −0.11513 (12) | 0.30880 (6) | 0.0422 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.01944 (18) | 0.01858 (18) | 0.0300 (2) | 0.00088 (14) | −0.00031 (15) | −0.00206 (15) |
N2 | 0.0232 (12) | 0.0234 (12) | 0.0401 (14) | 0.0011 (10) | 0.0020 (11) | −0.0046 (10) |
C3 | 0.0250 (14) | 0.0275 (14) | 0.0265 (15) | −0.0053 (11) | 0.0027 (11) | −0.0044 (12) |
S4 | 0.0518 (5) | 0.0240 (4) | 0.0528 (5) | 0.0076 (3) | 0.0060 (4) | −0.0073 (3) |
N5 | 0.0226 (12) | 0.0230 (11) | 0.0333 (13) | 0.0003 (9) | 0.0014 (10) | −0.0017 (10) |
C6 | 0.0194 (13) | 0.0225 (13) | 0.0308 (15) | −0.0060 (11) | −0.0024 (11) | 0.0029 (12) |
S7 | 0.0284 (4) | 0.0375 (4) | 0.0568 (5) | 0.0007 (3) | 0.0065 (4) | −0.0201 (4) |
N8 | 0.0225 (12) | 0.0198 (11) | 0.0293 (12) | −0.0004 (9) | −0.0007 (10) | −0.0009 (9) |
C9 | 0.0294 (15) | 0.0218 (13) | 0.0321 (15) | −0.0013 (11) | −0.0051 (12) | 0.0008 (12) |
C10 | 0.0267 (15) | 0.0224 (13) | 0.0325 (15) | 0.0056 (11) | −0.0016 (12) | −0.0029 (12) |
C11 | 0.0230 (14) | 0.0275 (14) | 0.0269 (14) | −0.0006 (11) | 0.0010 (11) | −0.0011 (12) |
C12 | 0.0286 (15) | 0.0200 (13) | 0.0459 (17) | −0.0014 (11) | −0.0063 (13) | −0.0051 (12) |
C13 | 0.0277 (15) | 0.0225 (13) | 0.0429 (17) | 0.0032 (11) | −0.0060 (13) | −0.0022 (12) |
C14 | 0.0271 (15) | 0.0350 (16) | 0.0364 (16) | 0.0026 (13) | −0.0002 (13) | −0.0099 (13) |
C15 | 0.0362 (17) | 0.0373 (16) | 0.052 (2) | 0.0065 (14) | −0.0148 (15) | −0.0069 (15) |
O16 | 0.0371 (13) | 0.0337 (12) | 0.0867 (17) | −0.0055 (9) | −0.0227 (12) | −0.0067 (11) |
N17 | 0.0220 (12) | 0.0223 (11) | 0.0280 (12) | −0.0004 (9) | −0.0002 (10) | −0.0002 (10) |
C18 | 0.0243 (15) | 0.0279 (14) | 0.0318 (16) | 0.0006 (11) | 0.0002 (12) | 0.0020 (12) |
C19 | 0.0261 (15) | 0.0253 (14) | 0.0344 (16) | −0.0029 (11) | −0.0047 (12) | −0.0025 (12) |
C20 | 0.0219 (14) | 0.0272 (13) | 0.0306 (15) | −0.0014 (11) | −0.0014 (12) | 0.0086 (12) |
C21 | 0.0216 (14) | 0.0310 (14) | 0.0324 (15) | 0.0031 (11) | 0.0036 (11) | 0.0022 (13) |
C22 | 0.0254 (14) | 0.0275 (14) | 0.0286 (15) | 0.0002 (11) | 0.0014 (12) | 0.0014 (12) |
C23 | 0.0242 (15) | 0.0388 (16) | 0.0362 (16) | −0.0022 (13) | −0.0026 (12) | 0.0055 (14) |
C24 | 0.0280 (17) | 0.058 (2) | 0.057 (2) | −0.0090 (15) | −0.0049 (15) | −0.0119 (17) |
O25 | 0.0237 (11) | 0.0491 (12) | 0.0683 (15) | 0.0035 (10) | −0.0051 (10) | −0.0026 (11) |
N26 | 0.0231 (12) | 0.0223 (11) | 0.0306 (13) | 0.0013 (9) | −0.0036 (10) | −0.0002 (10) |
C27 | 0.0281 (15) | 0.0273 (13) | 0.0331 (16) | −0.0006 (11) | −0.0049 (13) | −0.0052 (13) |
C28 | 0.0316 (16) | 0.0318 (15) | 0.0298 (16) | 0.0049 (12) | 0.0025 (12) | −0.0055 (13) |
C29 | 0.0270 (15) | 0.0257 (13) | 0.0292 (15) | 0.0068 (11) | −0.0010 (12) | 0.0018 (12) |
C30 | 0.0390 (17) | 0.0220 (13) | 0.0377 (17) | −0.0028 (12) | 0.0043 (13) | 0.0019 (13) |
C31 | 0.0372 (16) | 0.0232 (14) | 0.0281 (15) | 0.0024 (12) | 0.0035 (13) | −0.0001 (12) |
C32 | 0.0316 (16) | 0.0331 (15) | 0.0376 (17) | 0.0093 (13) | 0.0048 (13) | 0.0085 (14) |
C33 | 0.0343 (17) | 0.0467 (18) | 0.0404 (18) | −0.0040 (14) | 0.0068 (14) | 0.0092 (14) |
O34 | 0.0661 (16) | 0.0357 (11) | 0.0389 (12) | 0.0103 (10) | 0.0177 (11) | 0.0005 (10) |
N35 | 0.0196 (11) | 0.0203 (11) | 0.0317 (12) | −0.0007 (9) | −0.0037 (9) | −0.0009 (9) |
C36 | 0.0166 (13) | 0.0222 (13) | 0.0364 (16) | −0.0004 (10) | −0.0020 (12) | −0.0020 (12) |
C37 | 0.0172 (13) | 0.0200 (13) | 0.0322 (15) | 0.0020 (10) | 0.0008 (11) | −0.0036 (12) |
C38 | 0.0216 (14) | 0.0194 (12) | 0.0286 (14) | −0.0006 (10) | −0.0001 (11) | −0.0048 (11) |
C39 | 0.0171 (13) | 0.0229 (13) | 0.0340 (15) | 0.0000 (10) | −0.0032 (11) | 0.0015 (11) |
C40 | 0.0201 (13) | 0.0229 (13) | 0.0357 (16) | 0.0013 (10) | 0.0006 (12) | −0.0008 (12) |
C41 | 0.0290 (16) | 0.0253 (14) | 0.0348 (16) | 0.0055 (12) | 0.0027 (13) | −0.0022 (12) |
C42 | 0.0371 (17) | 0.0470 (17) | 0.0388 (18) | 0.0139 (14) | 0.0059 (14) | 0.0097 (15) |
O43 | 0.0306 (12) | 0.0510 (13) | 0.0451 (12) | 0.0086 (9) | 0.0115 (9) | 0.0136 (10) |
Co1—N2 | 2.067 (2) | C23—O25 | 1.223 (3) |
Co1—N5 | 2.072 (2) | C23—C24 | 1.485 (4) |
Co1—N35 | 2.153 (2) | C24—H24A | 0.9800 |
Co1—N8 | 2.183 (2) | C24—H24B | 0.9800 |
Co1—N26 | 2.205 (2) | C24—H24C | 0.9800 |
Co1—N17 | 2.224 (2) | N26—C27 | 1.341 (3) |
N2—C3 | 1.164 (3) | N26—C31 | 1.346 (3) |
C3—S4 | 1.629 (3) | C27—C28 | 1.375 (4) |
N5—C6 | 1.160 (3) | C27—H27 | 0.9500 |
C6—S7 | 1.628 (3) | C28—C29 | 1.386 (3) |
N8—C9 | 1.333 (3) | C28—H28 | 0.9500 |
N8—C13 | 1.343 (3) | C29—C30 | 1.383 (3) |
C9—C10 | 1.382 (3) | C29—C32 | 1.506 (4) |
C9—H9 | 0.9500 | C30—C31 | 1.382 (3) |
C10—C11 | 1.382 (3) | C30—H30 | 0.9500 |
C10—H10 | 0.9500 | C31—H31 | 0.9500 |
C11—C12 | 1.394 (3) | C32—O34 | 1.222 (3) |
C11—C14 | 1.501 (4) | C32—C33 | 1.494 (4) |
C12—C13 | 1.383 (3) | C33—H33A | 0.9800 |
C12—H12 | 0.9500 | C33—H33B | 0.9800 |
C13—H13 | 0.9500 | C33—H33C | 0.9800 |
C14—O16 | 1.211 (3) | N35—C36 | 1.348 (3) |
C14—C15 | 1.491 (4) | N35—C40 | 1.353 (3) |
C15—H15A | 0.9800 | C36—C37 | 1.370 (3) |
C15—H15B | 0.9800 | C36—H36 | 0.9500 |
C15—H15C | 0.9800 | C37—C38 | 1.394 (3) |
N17—C18 | 1.338 (3) | C37—H37 | 0.9500 |
N17—C22 | 1.345 (3) | C38—C39 | 1.387 (3) |
C18—C19 | 1.394 (3) | C38—C41 | 1.491 (4) |
C18—H18 | 0.9500 | C39—C40 | 1.369 (4) |
C19—C20 | 1.385 (3) | C39—H39 | 0.9500 |
C19—H19 | 0.9500 | C40—H40 | 0.9500 |
C20—C21 | 1.380 (4) | C41—O43 | 1.221 (3) |
C20—C23 | 1.514 (4) | C41—C42 | 1.500 (4) |
C21—C22 | 1.382 (3) | C42—H42A | 0.9800 |
C21—H21 | 0.9500 | C42—H42B | 0.9800 |
C22—H22 | 0.9500 | C42—H42C | 0.9800 |
N2—Co1—N5 | 177.75 (9) | O25—C23—C24 | 123.2 (3) |
N2—Co1—N35 | 90.75 (8) | O25—C23—C20 | 118.4 (2) |
N5—Co1—N35 | 87.31 (8) | C24—C23—C20 | 118.4 (2) |
N2—Co1—N8 | 91.94 (8) | C23—C24—H24A | 109.5 |
N5—Co1—N8 | 89.23 (8) | C23—C24—H24B | 109.5 |
N35—Co1—N8 | 91.33 (8) | H24A—C24—H24B | 109.5 |
N2—Co1—N26 | 90.75 (8) | C23—C24—H24C | 109.5 |
N5—Co1—N26 | 91.10 (8) | H24A—C24—H24C | 109.5 |
N35—Co1—N26 | 175.12 (8) | H24B—C24—H24C | 109.5 |
N8—Co1—N26 | 93.26 (7) | C27—N26—C31 | 116.4 (2) |
N2—Co1—N17 | 89.71 (8) | C27—N26—Co1 | 124.08 (16) |
N5—Co1—N17 | 89.23 (8) | C31—N26—Co1 | 118.01 (16) |
N35—Co1—N17 | 91.99 (7) | N26—C27—C28 | 123.5 (2) |
N8—Co1—N17 | 176.27 (7) | N26—C27—H27 | 118.2 |
N26—Co1—N17 | 83.37 (7) | C28—C27—H27 | 118.2 |
C3—N2—Co1 | 163.3 (2) | C27—C28—C29 | 119.7 (2) |
N2—C3—S4 | 178.1 (2) | C27—C28—H28 | 120.1 |
C6—N5—Co1 | 163.64 (19) | C29—C28—H28 | 120.1 |
N5—C6—S7 | 179.2 (2) | C30—C29—C28 | 117.4 (2) |
C9—N8—C13 | 117.2 (2) | C30—C29—C32 | 122.4 (2) |
C9—N8—Co1 | 121.14 (16) | C28—C29—C32 | 120.1 (2) |
C13—N8—Co1 | 121.57 (16) | C29—C30—C31 | 119.3 (2) |
N8—C9—C10 | 123.5 (2) | C29—C30—H30 | 120.3 |
N8—C9—H9 | 118.2 | C31—C30—H30 | 120.3 |
C10—C9—H9 | 118.2 | N26—C31—C30 | 123.5 (2) |
C11—C10—C9 | 119.4 (2) | N26—C31—H31 | 118.2 |
C11—C10—H10 | 120.3 | C30—C31—H31 | 118.2 |
C9—C10—H10 | 120.3 | O34—C32—C33 | 122.4 (2) |
C10—C11—C12 | 117.6 (2) | O34—C32—C29 | 119.3 (2) |
C10—C11—C14 | 122.6 (2) | C33—C32—C29 | 118.3 (2) |
C12—C11—C14 | 119.8 (2) | C32—C33—H33A | 109.5 |
C13—C12—C11 | 119.3 (2) | C32—C33—H33B | 109.5 |
C13—C12—H12 | 120.4 | H33A—C33—H33B | 109.5 |
C11—C12—H12 | 120.4 | C32—C33—H33C | 109.5 |
N8—C13—C12 | 122.9 (2) | H33A—C33—H33C | 109.5 |
N8—C13—H13 | 118.5 | H33B—C33—H33C | 109.5 |
C12—C13—H13 | 118.5 | C36—N35—C40 | 117.5 (2) |
O16—C14—C15 | 121.1 (3) | C36—N35—Co1 | 122.71 (16) |
O16—C14—C11 | 119.9 (2) | C40—N35—Co1 | 119.70 (17) |
C15—C14—C11 | 118.9 (2) | N35—C36—C37 | 122.5 (2) |
C14—C15—H15A | 109.5 | N35—C36—H36 | 118.8 |
C14—C15—H15B | 109.5 | C37—C36—H36 | 118.8 |
H15A—C15—H15B | 109.5 | C36—C37—C38 | 119.8 (2) |
C14—C15—H15C | 109.5 | C36—C37—H37 | 120.1 |
H15A—C15—H15C | 109.5 | C38—C37—H37 | 120.1 |
H15B—C15—H15C | 109.5 | C39—C38—C37 | 117.8 (2) |
C18—N17—C22 | 117.3 (2) | C39—C38—C41 | 122.8 (2) |
C18—N17—Co1 | 121.90 (16) | C37—C38—C41 | 119.4 (2) |
C22—N17—Co1 | 120.58 (16) | C40—C39—C38 | 119.3 (2) |
N17—C18—C19 | 123.5 (2) | C40—C39—H39 | 120.3 |
N17—C18—H18 | 118.2 | C38—C39—H39 | 120.3 |
C19—C18—H18 | 118.2 | N35—C40—C39 | 123.0 (2) |
C20—C19—C18 | 118.5 (2) | N35—C40—H40 | 118.5 |
C20—C19—H19 | 120.8 | C39—C40—H40 | 118.5 |
C18—C19—H19 | 120.8 | O43—C41—C38 | 119.8 (2) |
C21—C20—C19 | 118.2 (2) | O43—C41—C42 | 121.2 (2) |
C21—C20—C23 | 119.4 (2) | C38—C41—C42 | 119.0 (2) |
C19—C20—C23 | 122.4 (2) | C41—C42—H42A | 109.5 |
C22—C21—C20 | 119.9 (2) | C41—C42—H42B | 109.5 |
C22—C21—H21 | 120.0 | H42A—C42—H42B | 109.5 |
C20—C21—H21 | 120.0 | C41—C42—H42C | 109.5 |
N17—C22—C21 | 122.5 (2) | H42A—C42—H42C | 109.5 |
N17—C22—H22 | 118.7 | H42B—C42—H42C | 109.5 |
C21—C22—H22 | 118.7 |
Experimental details
Crystal data | |
Chemical formula | [Co(NCS)2(C7H7NO)4] |
Mr | 659.63 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 110 |
a, b, c (Å) | 11.9180 (2), 15.9700 (2), 33.1930 (6) |
V (Å3) | 6317.64 (17) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 0.72 |
Crystal size (mm) | 0.25 × 0.20 × 0.10 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SORTAV; Blessing, 1995) |
Tmin, Tmax | 0.841, 0.932 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14852, 7506, 4541 |
Rint | 0.063 |
(sin θ/λ)max (Å−1) | 0.658 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.115, 1.02 |
No. of reflections | 7506 |
No. of parameters | 392 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.38, −0.39 |
Computer programs: COLLECT (Nonius B.V., 1999), DENZO (Otwinowski, 1985), SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), ORTEPIII (Burnett & Johnson, 1996), SHELXL97.
It has been demonstrated during the last few decades that halido or pseudo-halido complexes of cobalt(II) that contain pyridines and substituted pyridines undergo a series of interesting solid-state reactions (Agnew et al., 1974; Liptay et al., 1992). These complexes also exhibited selective enclathration of other species (Schaeffer et al., 1957). Extensive differential scanning calorimetry and optical microscopic studies were carried out on the solid-state reactions of cobalt(II) pseudo-halido complexes containing substituted pyridines (Agnew & Brown, 1974). In the observed structure, the central Co atom is six-coordinate to four equatorial pyridyl donors and two axial thiocyanates, forming an octahedral structure.