metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 6| June 2012| Pages m733-m734

A triclinic polymorph of poly[[bis­­[μ-1,2-bis­­(pyridin-4-yl)ethene-κ2N:N′]bis­­(thio­cyanato-κN)cobalt(II)] 1,2-bis­­(pyridin-4-yl)ethene monosolvate]

aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany
*Correspondence e-mail: swoehlert@ac.uni-kiel.de

(Received 20 April 2012; accepted 27 April 2012; online 5 May 2012)

In the crystal structure of the title compound, [Co(NCS)2(C12H10N2)2]·C12H10N2, the CoII cations are octa­hedrally coordinated by two terminally N-bonded thio­cyanate anions and four 1,2-bis­(pyridin-4-yl)ethene (bpe) ligands. The asymmetric unit consists of three crystallographically independent CoII cations, six thio­cyanate anions and six coordinating bpe ligands in general positions. Additionally, three non-coordin­ating bpe ligands are present in the asymmetric unit with two of them located on a center of inversion. The CoII cations are connected by the bpe ligands into layers parallel to the bc plane. The crystal investigated was non-merohedrically twinned, with a fractional contribution of 0.261 (2) for the minor domain.

Related literature

For background to this work see: Boeckmann & Näther (2010[Boeckmann, J. & Näther, C. (2010). Dalton Trans. 39, 1119-1126.]), Wriedt et al. (2009[Wriedt, M., Jess, I. & Näther, C. (2009). Eur. J. Inorg. Chem. pp. 1406-1413.]). For the monoclinic polymorph of the title compound, see: Wöhlert et al. (2011[Wöhlert, S., Boeckmann, J., Wriedt, M. & Näther, C. (2011). Angew. Chem. Int. Ed., 50, 6920-6923.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(NCS)2(C12H10N2)2]·C12H10N2

  • Mr = 721.75

  • Triclinic, [P \overline 1]

  • a = 13.7954 (14) Å

  • b = 13.8916 (13) Å

  • c = 27.848 (2) Å

  • α = 99.892 (10)°

  • β = 90.547 (11)°

  • γ = 91.269 (11)°

  • V = 5255.7 (8) Å3

  • Z = 6

  • Mo Kα radiation

  • μ = 0.65 mm−1

  • T = 170 K

  • 0.3 × 0.2 × 0.2 mm

Data collection
  • Stoe IPDS-1 diffractometer

  • 15899 measured reflections

  • 15899 independent reflections

  • 11067 reflections with I > 2σ(I)

  • θmax = 24.1°

Refinement
  • R[F2 > 2σ(F2)] = 0.054

  • wR(F2) = 0.166

  • S = 1.03

  • 15899 reflections

  • 1326 parameters

  • H-atom parameters constrained

  • Δρmax = 0.84 e Å−3

  • Δρmin = −0.68 e Å−3

Data collection: X-AREA (Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA and X-RED32. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-RED32 (Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA and X-RED32. Stoe & Cie, Darmstadt, Germany.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: XP (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and DIAMOND (Brandenburg, 2011[Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: CIFTAB (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information


Comment top

Recently we have reported on our investigations on the synthesis, structures and properties of new coordination polymers based on paramagnetic transition metal and N-donor co-ligands, in which the transition metal anions are linked into chains by thiocyanato anions (Wriedt et al., 2009 and Boeckmann & Näther, 2010 as well as Wöhlert et al., 2011). In the course of these investigations we have reported on a cobalt-thiocyanato compound with bpe (1,2-bis(pyridine-4-yl)ethyene) as ligand that shows a slow relaxation of the magnetization (Wöhlert et al., 2011). This compound can be prepared by thermal decomposition of the precursor [bis(thiocyanato-N)-bis(1,2-bis(pyridine-4-yl)ethyene-N)-cobalt(II)]-1,2-bis(pyridine-4-yl)ethyene-solvate. In further investigations we have obtained a second polymorphic modification of this precursor which was characterized by single crystal X-ray diffraction.

In the crystal structure of the title compound, each of the three cobalt(II) cation is coordinated by two terminally N-bonded thiocyanato anions and four bpe ligands (Fig. 1–4). The CoN6 octahedrons are slightly distorted with distances ranging from 2.051 (5) Å to 2.245 (3). The angles arround the metal atoms are in the range of 87.39 ° to 178.91 (15) °. The cobalt(II) cations are linked by the bpe ligands into chains that are further connected into layers by additional coligands (Fig. 5). The layers are stacked in order that channels are formed, in which non-coordinated bpe molecules are located. The Co—Co distances within the chains are 13.7954 (16) Å and 13.8916 (15) Å.

Related literature top

For background to this work see: Boeckmann & Näther (2010), Wriedt et al. (2009); Wöhlert et al. (2011).

Experimental top

Cobalt thiocyanate (Co(NCS)2) and 1,2-bis(pyridine-4-yl)ethyene (bpe) were obtained from Alfa Aesar, Sigma Aldrich respectively. All chemicals were used without further purification. 0.15 mmol (28.9 mg) Co(NCS)2 and 0.6 mmol (108.4 mg) bpe were reacted with 1 ml H2O in a closed test-tube at 120 ° C for three days. On cooling orange block-shaped single crystals of the title compound were obtained.

Refinement top

H atoms were positioned with idealized geometry and were refined isotropically with Uiso(H) = 1.2Ueq(C) and C—H distances of 0.95 Å using a riding model. The crystal investigated was non-merohedrically twinned. The twin matrix was calculated from the orientation matrices of both individuals and afterwards a new HKL file in HKLF-5 format was generated and the structure was refined using the HKLF-5 option in SHELXL-97 [BASF parameter: 0.261 (2)].

Computing details top

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-RED32 (Stoe & Cie, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011); software used to prepare material for publication: CIFTAB (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. : Environment of Co1 with labelling and displacement ellipsoids drawn at the 50 % probability level. Symmetry codes: i = x, y-1, z; ii = x+1, y, z. For clarity the non-coordinated bpe ligands are omitted.
[Figure 2] Fig. 2. : Environment of Co2 with labelling and displacement ellipsoids drawn at the 50 % probability level. Symmetry codes: ii = x+1, y, z; iii = x, y+1, z. For clarity the non-coordinated bpe ligands are omitted.
[Figure 3] Fig. 3. : Environment of Co3 with labelling and displacement ellipsoids drawn at the 50 % probability level. Symmetry codes: i = x, y-1, z; iv = x-1, y, z. For clarity the non-coordinated bpe ligands are omitted.
[Figure 4] Fig. 4. : View of the non-coordinated 1,2-bis(pyridine-4-yl)ethyene ligands with labelling and displacement ellipsoids drawn at the 50 % probability level. Symmetry codes: v = -x+1, -y+2, -z+1; vi = -x+1, -y, -z.
[Figure 5] Fig. 5. : Crystal structure of the title compound with view approximately along the crystallographic c-axis. The non-coordinated bpe ligands are omitted for clarity.
Poly[[bis[µ-1,2-bis(pyridin-4-yl)ethene- κ2N:N']bis(thiocyanato-κN)cobalt(II)] 1,2-bis(pyridin-4-yl)ethene monosolvate] top
Crystal data top
[Co(NCS)2(C12H10N2)2]·C12H10N2Z = 6
Mr = 721.75F(000) = 2238
Triclinic, P1Dx = 1.368 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 13.7954 (14) ÅCell parameters from 15899 reflections
b = 13.8916 (13) Åθ = 1.6–24.1°
c = 27.848 (2) ŵ = 0.65 mm1
α = 99.892 (10)°T = 170 K
β = 90.547 (11)°Block, orange
γ = 91.269 (11)°0.3 × 0.2 × 0.2 mm
V = 5255.7 (8) Å3
Data collection top
Stoe IPDS-1
diffractometer
11067 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 24.1°, θmin = 1.6°
phi scansh = 1515
15899 measured reflectionsk = 1515
15899 independent reflectionsl = 3030
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.054H-atom parameters constrained
wR(F2) = 0.166 w = 1/[σ2(Fo2) + (0.1032P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
15899 reflectionsΔρmax = 0.84 e Å3
1326 parametersΔρmin = 0.68 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0054 (5)
Crystal data top
[Co(NCS)2(C12H10N2)2]·C12H10N2γ = 91.269 (11)°
Mr = 721.75V = 5255.7 (8) Å3
Triclinic, P1Z = 6
a = 13.7954 (14) ÅMo Kα radiation
b = 13.8916 (13) ŵ = 0.65 mm1
c = 27.848 (2) ÅT = 170 K
α = 99.892 (10)°0.3 × 0.2 × 0.2 mm
β = 90.547 (11)°
Data collection top
Stoe IPDS-1
diffractometer
11067 reflections with I > 2σ(I)
15899 measured reflectionsRint = 0.000
15899 independent reflectionsθmax = 24.1°
Refinement top
R[F2 > 2σ(F2)] = 0.0540 restraints
wR(F2) = 0.166H-atom parameters constrained
S = 1.03Δρmax = 0.84 e Å3
15899 reflectionsΔρmin = 0.68 e Å3
1326 parameters
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.10026 (4)0.52321 (4)0.24971 (2)0.01071 (17)
N10.1118 (3)0.6860 (3)0.25417 (14)0.0120 (8)
C10.0997 (3)0.7288 (3)0.21527 (19)0.0179 (11)
H10.09130.68800.18440.021*
C20.0988 (4)0.8297 (3)0.21715 (19)0.0207 (11)
H20.08790.85620.18840.025*
C30.1138 (3)0.8907 (3)0.26146 (18)0.0155 (10)
C40.1286 (4)0.8463 (3)0.30218 (19)0.0218 (11)
H40.14010.88540.33330.026*
C50.1265 (3)0.7457 (3)0.29740 (18)0.0179 (11)
H50.13590.71730.32570.021*
C60.1144 (4)0.9989 (3)0.2683 (2)0.0236 (12)
H60.13301.03380.29950.028*
C70.0915 (4)1.0499 (3)0.23507 (19)0.0207 (11)
H70.07111.01450.20420.025*
C80.0941 (3)1.1579 (3)0.24068 (19)0.0173 (11)
C90.1088 (4)1.2200 (3)0.28521 (19)0.0196 (11)
H90.11901.19420.31430.024*
C100.1083 (3)1.3204 (3)0.28622 (18)0.0179 (11)
H100.11781.36190.31680.022*
C110.0818 (3)1.3017 (3)0.20417 (18)0.0174 (11)
H110.07231.32920.17550.021*
C120.0809 (4)1.2006 (3)0.19969 (19)0.0199 (11)
H120.07141.16080.16860.024*
N20.0951 (3)1.3627 (3)0.24665 (14)0.0132 (8)
N210.0598 (3)0.5304 (3)0.25350 (15)0.0145 (9)
C210.1180 (3)0.4489 (3)0.24838 (18)0.0161 (10)
H210.08790.38740.24110.019*
C220.2179 (3)0.4489 (4)0.2530 (2)0.0214 (12)
H220.25400.38900.24970.026*
C230.2647 (3)0.5377 (3)0.26261 (19)0.0159 (11)
C240.2043 (3)0.6227 (3)0.26913 (19)0.0197 (11)
H240.23200.68540.27720.024*
C250.1057 (3)0.6149 (3)0.26386 (17)0.0162 (10)
H250.06770.67360.26790.019*
C260.3699 (4)0.5482 (3)0.26806 (19)0.0206 (11)
H260.39340.60470.28830.025*
C270.4348 (3)0.4805 (4)0.2454 (2)0.0202 (11)
H270.41130.42190.22690.024*
C280.5394 (4)0.4938 (3)0.24813 (19)0.0183 (11)
C290.5996 (4)0.4351 (4)0.2128 (2)0.0217 (11)
H290.57250.38740.18840.026*
C300.6986 (3)0.4484 (4)0.2146 (2)0.0220 (12)
H300.73810.40970.19020.026*
C310.6837 (3)0.5666 (3)0.28201 (19)0.0181 (11)
H310.71330.61260.30630.022*
C320.5844 (3)0.5598 (3)0.2831 (2)0.0211 (11)
H320.54700.60030.30780.025*
N220.7414 (3)0.5108 (3)0.24776 (17)0.0262 (11)
S2110.15370 (12)0.51234 (11)0.07889 (6)0.0344 (4)
C2110.1200 (3)0.5073 (3)0.1342 (2)0.0183 (11)
N2110.0969 (3)0.5049 (3)0.17461 (16)0.0176 (9)
S2210.18076 (12)0.54030 (11)0.41796 (5)0.0343 (4)
C2210.1363 (3)0.5428 (3)0.36419 (19)0.0152 (10)
N2210.1052 (3)0.5440 (3)0.32487 (16)0.0160 (9)
Co20.90452 (4)0.17932 (4)0.41476 (2)0.01004 (17)
N410.9056 (3)0.0185 (3)0.41222 (14)0.0125 (8)
C410.9135 (4)0.0417 (3)0.36949 (19)0.0196 (11)
H410.91880.01370.34080.024*
C420.9142 (4)0.1420 (3)0.36485 (19)0.0220 (12)
H420.92040.18110.33360.026*
C430.9059 (3)0.1863 (3)0.40576 (18)0.0155 (10)
C440.8979 (4)0.1246 (3)0.45000 (19)0.0191 (11)
H440.89310.15090.47920.023*
C450.8968 (4)0.0246 (3)0.45181 (19)0.0191 (11)
H450.88940.01590.48260.023*
C460.9080 (4)0.2937 (3)0.3996 (2)0.0218 (11)
H460.92060.32780.36780.026*
C470.8941 (4)0.3470 (3)0.43370 (19)0.0219 (11)
H470.88310.31310.46580.026*
C480.8939 (3)0.4531 (3)0.42685 (18)0.0166 (11)
C490.8956 (4)0.5146 (3)0.38202 (19)0.0184 (11)
H490.89630.48760.35290.022*
C500.8964 (3)0.6153 (3)0.37934 (18)0.0172 (11)
H500.89620.65520.34800.021*
C510.8946 (4)0.6003 (3)0.46190 (19)0.0197 (11)
H510.89440.62940.49040.024*
C520.8923 (4)0.4995 (3)0.46770 (18)0.0215 (11)
H520.88950.46160.49950.026*
N420.8973 (3)0.6592 (3)0.41862 (14)0.0138 (8)
N610.7475 (3)0.1700 (3)0.41465 (16)0.0138 (9)
C610.6980 (3)0.1061 (3)0.38163 (19)0.0182 (11)
H610.73400.06500.35770.022*
C620.5987 (3)0.0955 (4)0.3798 (2)0.0239 (12)
H620.56810.04760.35560.029*
C630.5432 (3)0.1557 (4)0.4137 (2)0.0209 (11)
C640.5928 (3)0.2229 (4)0.44899 (19)0.0219 (11)
H640.55830.26450.47330.026*
C650.6929 (3)0.2279 (3)0.44797 (19)0.0186 (11)
H650.72570.27450.47200.022*
C660.4368 (4)0.1433 (4)0.4108 (2)0.0238 (12)
H660.40980.08420.39300.029*
C670.3763 (4)0.2119 (4)0.4321 (2)0.0245 (12)
H670.40300.26930.45170.029*
C680.2702 (4)0.2011 (4)0.42626 (19)0.0212 (12)
C690.2193 (4)0.1102 (4)0.4201 (2)0.0256 (12)
H690.25380.05160.41960.031*
C700.1206 (3)0.1066 (3)0.41500 (19)0.0189 (11)
H700.08870.04430.41010.023*
C710.1145 (3)0.2726 (3)0.42231 (19)0.0188 (11)
H710.07870.33030.42250.023*
C720.2137 (3)0.2816 (4)0.4281 (2)0.0245 (12)
H720.24370.34480.43340.029*
N620.0656 (3)0.1860 (3)0.41647 (16)0.0178 (9)
S2310.82516 (10)0.17983 (10)0.24772 (5)0.0283 (3)
C2310.8693 (3)0.1679 (3)0.30103 (19)0.0154 (10)
N2310.9001 (3)0.1602 (3)0.33914 (16)0.0169 (9)
S2410.81912 (11)0.16166 (11)0.57629 (6)0.0338 (4)
C2410.8690 (3)0.1861 (3)0.52692 (19)0.0170 (11)
N2410.9043 (3)0.2000 (3)0.49035 (15)0.0156 (9)
Co30.88767 (4)0.85152 (4)0.08589 (2)0.01137 (17)
N811.0487 (3)0.8598 (3)0.09040 (15)0.0175 (9)
C811.0964 (3)0.9469 (3)0.09791 (19)0.0186 (11)
H811.05981.00450.09960.022*
C821.1958 (4)0.9568 (4)0.1032 (2)0.0250 (12)
H821.22551.02010.10990.030*
C831.2534 (3)0.8730 (4)0.0988 (2)0.0199 (11)
C841.2028 (3)0.7837 (4)0.09070 (19)0.0186 (11)
H841.23730.72460.08830.022*
C851.1032 (3)0.7804 (3)0.08619 (18)0.0182 (11)
H851.07130.71810.07970.022*
C861.3589 (3)0.8843 (3)0.1037 (2)0.0205 (11)
H861.38520.94160.12350.025*
C871.4200 (4)0.8179 (4)0.0818 (2)0.0240 (12)
H871.39240.75970.06340.029*
C881.5268 (3)0.8274 (4)0.0837 (2)0.0188 (11)
C891.5807 (3)0.7675 (3)0.0509 (2)0.0216 (12)
H891.54950.71950.02700.026*
C901.6808 (3)0.7766 (3)0.05236 (19)0.0203 (11)
H901.71660.73280.02960.024*
C911.6758 (3)0.9026 (3)0.11739 (19)0.0194 (11)
H911.70840.94900.14160.023*
C921.5760 (3)0.8987 (4)0.11799 (19)0.0206 (11)
H921.54120.94300.14100.025*
N821.7306 (3)0.8451 (3)0.08478 (15)0.0148 (9)
N1010.8795 (3)1.0095 (3)0.08072 (14)0.0132 (8)
C1010.8808 (4)1.0387 (3)0.0373 (2)0.0231 (12)
H1010.88190.99040.00870.028*
C1020.8807 (4)1.1355 (4)0.0324 (2)0.0284 (13)
H1020.88161.15230.00070.034*
C1030.8791 (3)1.2093 (3)0.07311 (19)0.0184 (11)
C1040.8751 (4)1.1785 (3)0.11815 (19)0.0196 (11)
H1040.87171.22510.14730.024*
C1050.8760 (3)1.0795 (3)0.12013 (18)0.0168 (10)
H1050.87421.06030.15130.020*
C1060.8817 (4)1.3122 (3)0.0672 (2)0.0254 (12)
H1060.89251.32500.03530.030*
C1070.8705 (4)1.3891 (3)0.1020 (2)0.0224 (11)
H1070.85921.37660.13390.027*
C1080.8741 (3)1.4911 (3)0.09558 (19)0.0181 (11)
C1090.8907 (4)1.5237 (3)0.0520 (2)0.0234 (12)
H1090.89971.47760.02310.028*
C1100.8943 (4)1.6224 (4)0.05031 (19)0.0216 (11)
H1100.90471.64200.01970.026*
C1110.8670 (4)1.6611 (3)0.13199 (19)0.0213 (11)
H1110.85851.70860.16050.026*
C1120.8614 (4)1.5637 (3)0.1361 (2)0.0242 (12)
H1120.84881.54580.16690.029*
N1020.8839 (3)1.6922 (3)0.08957 (15)0.0144 (9)
S2510.83392 (13)0.78391 (12)0.08676 (6)0.0402 (4)
C2510.8672 (4)0.8014 (3)0.0298 (2)0.0184 (11)
N2510.8906 (3)0.8150 (3)0.01135 (17)0.0193 (9)
S2610.81790 (12)0.88533 (11)0.25419 (5)0.0355 (4)
C2610.8590 (3)0.8888 (3)0.20008 (19)0.0159 (10)
N2610.8880 (3)0.8892 (3)0.16113 (16)0.0166 (9)
N1210.4626 (4)0.0743 (4)0.2029 (2)0.0469 (14)
C1210.5444 (5)0.1086 (5)0.2258 (2)0.0438 (17)
H1210.60280.07720.21530.053*
C1220.5505 (4)0.1869 (4)0.2639 (2)0.0317 (14)
H1220.61190.20950.27770.038*
C1230.4659 (4)0.2328 (4)0.2822 (2)0.0292 (13)
C1240.3805 (5)0.1963 (5)0.2585 (3)0.0473 (18)
H1240.32050.22510.26850.057*
C1250.3824 (5)0.1188 (5)0.2206 (3)0.0532 (19)
H1250.32220.09500.20590.064*
C1260.4638 (4)0.3162 (4)0.3228 (2)0.0287 (13)
H1260.40230.34320.33090.034*
C1270.5391 (4)0.3571 (4)0.3491 (2)0.0296 (13)
H1270.60090.33050.34080.035*
C1280.5363 (4)0.4401 (4)0.3898 (2)0.0310 (13)
C1290.4512 (4)0.4870 (4)0.4055 (2)0.0291 (13)
H1290.39080.46560.39020.035*
C1300.4557 (4)0.5650 (4)0.4436 (2)0.0378 (15)
H1300.39710.59720.45290.045*
C1310.6171 (5)0.5531 (5)0.4530 (3)0.0484 (18)
H1310.67640.57540.46920.058*
C1320.6201 (4)0.4757 (4)0.4149 (2)0.0395 (15)
H1320.68030.44650.40580.047*
N1220.5362 (4)0.5986 (4)0.4685 (2)0.0426 (13)
N1410.5148 (5)0.4053 (4)0.0353 (2)0.0557 (16)
C1410.4331 (5)0.4408 (5)0.0584 (3)0.0479 (18)
H1410.37290.40980.04750.057*
C1420.4319 (5)0.5180 (5)0.0962 (2)0.0415 (16)
H1420.37200.53990.11010.050*
C1430.5180 (4)0.5642 (4)0.1142 (2)0.0324 (14)
C1440.6017 (5)0.5289 (5)0.0902 (3)0.0474 (17)
H1440.66280.55880.10020.057*
C1450.5966 (5)0.4511 (5)0.0521 (3)0.058 (2)
H1450.65540.42910.03690.070*
C1460.5247 (4)0.6472 (4)0.1545 (2)0.0344 (14)
H1460.58760.67450.16290.041*
C1470.4519 (4)0.6879 (4)0.1802 (2)0.0302 (13)
H1470.38890.66090.17180.036*
C1480.4596 (4)0.7711 (4)0.2206 (2)0.0318 (14)
C1490.3772 (5)0.8105 (4)0.2447 (2)0.0425 (16)
H1490.31490.78340.23470.051*
C1500.3855 (5)0.8881 (5)0.2827 (3)0.058 (2)
H1500.32780.91220.29830.069*
C1510.5490 (5)0.8926 (5)0.2753 (3)0.0464 (18)
H1510.61040.92100.28600.056*
C1520.5480 (5)0.8170 (5)0.2377 (3)0.0417 (16)
H1520.60710.79490.22290.050*
N1420.4695 (4)0.9316 (4)0.2990 (2)0.0459 (14)
N1610.5418 (4)0.7374 (4)0.3692 (2)0.0466 (14)
C1610.4587 (5)0.7713 (5)0.3900 (3)0.0468 (17)
H1610.39960.74000.37750.056*
C1620.4540 (4)0.8481 (4)0.4279 (2)0.0367 (15)
H1620.39270.86810.44070.044*
C1630.5371 (4)0.8967 (4)0.4479 (2)0.0286 (13)
C1640.6231 (5)0.8625 (5)0.4268 (3)0.0476 (18)
H1640.68310.89330.43840.057*
C1650.6219 (5)0.7843 (5)0.3892 (3)0.057 (2)
H1650.68250.76170.37640.068*
C1660.5390 (4)0.9801 (4)0.4884 (2)0.0297 (13)
H1660.60061.00800.49910.036*
N1710.5214 (4)0.2624 (4)0.1331 (2)0.0447 (14)
C1710.4422 (5)0.2247 (5)0.1081 (3)0.0441 (17)
H1710.38210.25450.11690.053*
C1720.4410 (4)0.1468 (4)0.0709 (2)0.0375 (15)
H1720.38120.12200.05600.045*
C1730.5280 (4)0.1034 (4)0.0548 (2)0.0313 (14)
C1740.6106 (5)0.1431 (5)0.0799 (3)0.0467 (18)
H1740.67210.11700.07070.056*
C1750.6042 (5)0.2210 (5)0.1183 (3)0.0502 (19)
H1750.66230.24590.13500.060*
C1760.5358 (4)0.0209 (4)0.0139 (2)0.0324 (13)
H1760.59860.00430.00720.039*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0127 (3)0.0085 (3)0.0109 (4)0.0014 (2)0.0004 (2)0.0019 (2)
N10.0120 (19)0.0076 (18)0.017 (2)0.0027 (14)0.0005 (16)0.0045 (16)
C10.026 (3)0.014 (2)0.014 (3)0.001 (2)0.002 (2)0.003 (2)
C20.032 (3)0.015 (2)0.017 (3)0.002 (2)0.003 (2)0.010 (2)
C30.026 (3)0.008 (2)0.014 (3)0.0035 (19)0.001 (2)0.0066 (19)
C40.036 (3)0.014 (2)0.016 (3)0.001 (2)0.000 (2)0.003 (2)
C50.026 (3)0.012 (2)0.016 (3)0.0013 (19)0.002 (2)0.005 (2)
C60.042 (3)0.010 (2)0.017 (3)0.000 (2)0.001 (2)0.002 (2)
C70.036 (3)0.005 (2)0.018 (3)0.002 (2)0.001 (2)0.003 (2)
C80.018 (2)0.014 (2)0.021 (3)0.0040 (19)0.006 (2)0.004 (2)
C90.031 (3)0.007 (2)0.023 (3)0.001 (2)0.002 (2)0.007 (2)
C100.028 (3)0.011 (2)0.014 (3)0.001 (2)0.002 (2)0.0008 (19)
C110.024 (3)0.011 (2)0.017 (3)0.0014 (19)0.001 (2)0.003 (2)
C120.033 (3)0.009 (2)0.015 (3)0.004 (2)0.000 (2)0.004 (2)
N20.0111 (19)0.0134 (19)0.016 (2)0.0003 (15)0.0010 (16)0.0044 (17)
N210.014 (2)0.014 (2)0.016 (2)0.0030 (16)0.0018 (16)0.0038 (17)
C210.018 (2)0.010 (2)0.019 (3)0.0040 (19)0.002 (2)0.0019 (19)
C220.019 (3)0.014 (3)0.032 (3)0.005 (2)0.001 (2)0.005 (2)
C230.019 (3)0.012 (2)0.017 (3)0.0066 (19)0.005 (2)0.006 (2)
C240.021 (3)0.011 (2)0.026 (3)0.0025 (19)0.001 (2)0.001 (2)
C250.019 (3)0.016 (2)0.011 (3)0.0051 (19)0.002 (2)0.0025 (19)
C260.022 (3)0.009 (2)0.028 (3)0.0033 (19)0.003 (2)0.006 (2)
C270.018 (3)0.016 (2)0.025 (3)0.001 (2)0.001 (2)0.001 (2)
C280.023 (3)0.014 (2)0.017 (3)0.009 (2)0.001 (2)0.003 (2)
C290.022 (3)0.017 (2)0.023 (3)0.001 (2)0.003 (2)0.007 (2)
C300.016 (3)0.019 (3)0.030 (3)0.002 (2)0.001 (2)0.001 (2)
C310.022 (3)0.008 (2)0.023 (3)0.0019 (19)0.003 (2)0.001 (2)
C320.018 (3)0.018 (3)0.025 (3)0.007 (2)0.001 (2)0.002 (2)
N220.010 (2)0.041 (3)0.024 (3)0.0029 (19)0.0029 (18)0.005 (2)
S2110.0493 (9)0.0353 (8)0.0207 (9)0.0045 (7)0.0094 (7)0.0092 (6)
C2110.020 (3)0.011 (2)0.024 (3)0.0006 (19)0.004 (2)0.002 (2)
N2110.023 (2)0.014 (2)0.015 (3)0.0004 (16)0.0011 (18)0.0004 (17)
S2210.0513 (9)0.0365 (8)0.0162 (8)0.0034 (7)0.0071 (7)0.0077 (6)
C2210.019 (2)0.008 (2)0.020 (3)0.0010 (18)0.003 (2)0.0054 (19)
N2210.021 (2)0.0109 (19)0.016 (3)0.0051 (16)0.0033 (18)0.0017 (16)
Co20.0119 (3)0.0073 (3)0.0106 (4)0.0013 (2)0.0008 (2)0.0007 (2)
N410.0119 (19)0.0128 (19)0.013 (2)0.0010 (15)0.0007 (16)0.0025 (16)
C410.028 (3)0.011 (2)0.021 (3)0.001 (2)0.000 (2)0.006 (2)
C420.043 (3)0.005 (2)0.016 (3)0.003 (2)0.000 (2)0.0029 (19)
C430.021 (3)0.013 (2)0.013 (3)0.0033 (19)0.001 (2)0.005 (2)
C440.032 (3)0.007 (2)0.019 (3)0.0035 (19)0.000 (2)0.005 (2)
C450.028 (3)0.015 (2)0.013 (3)0.002 (2)0.001 (2)0.000 (2)
C460.035 (3)0.012 (2)0.018 (3)0.001 (2)0.000 (2)0.000 (2)
C470.040 (3)0.010 (2)0.014 (3)0.002 (2)0.003 (2)0.002 (2)
C480.020 (3)0.009 (2)0.020 (3)0.0031 (18)0.003 (2)0.002 (2)
C490.028 (3)0.010 (2)0.018 (3)0.003 (2)0.001 (2)0.006 (2)
C500.025 (3)0.012 (2)0.013 (3)0.0025 (19)0.001 (2)0.0014 (19)
C510.029 (3)0.011 (2)0.019 (3)0.002 (2)0.000 (2)0.004 (2)
C520.042 (3)0.010 (2)0.011 (3)0.003 (2)0.003 (2)0.0032 (19)
N420.015 (2)0.0124 (19)0.013 (2)0.0021 (15)0.0025 (16)0.0018 (16)
N610.015 (2)0.0058 (19)0.020 (2)0.0043 (15)0.0032 (17)0.0006 (16)
C610.017 (3)0.013 (2)0.022 (3)0.0019 (19)0.002 (2)0.002 (2)
C620.016 (3)0.021 (3)0.030 (3)0.005 (2)0.002 (2)0.009 (2)
C630.015 (3)0.025 (3)0.024 (3)0.002 (2)0.000 (2)0.009 (2)
C640.016 (3)0.027 (3)0.021 (3)0.008 (2)0.004 (2)0.001 (2)
C650.018 (3)0.012 (2)0.023 (3)0.0051 (19)0.003 (2)0.002 (2)
C660.017 (3)0.023 (3)0.030 (3)0.002 (2)0.002 (2)0.001 (2)
C670.018 (3)0.023 (3)0.029 (3)0.005 (2)0.004 (2)0.004 (2)
C680.019 (3)0.028 (3)0.017 (3)0.001 (2)0.004 (2)0.005 (2)
C690.020 (3)0.027 (3)0.031 (4)0.004 (2)0.003 (2)0.008 (2)
C700.017 (3)0.017 (2)0.022 (3)0.006 (2)0.000 (2)0.004 (2)
C710.017 (3)0.018 (2)0.021 (3)0.001 (2)0.001 (2)0.003 (2)
C720.016 (3)0.018 (3)0.038 (4)0.003 (2)0.003 (2)0.002 (2)
N620.013 (2)0.023 (2)0.017 (2)0.0045 (17)0.0020 (17)0.0029 (18)
S2310.0384 (8)0.0299 (7)0.0178 (8)0.0002 (6)0.0055 (6)0.0077 (6)
C2310.018 (2)0.011 (2)0.016 (3)0.0028 (18)0.006 (2)0.0026 (19)
N2310.022 (2)0.011 (2)0.017 (3)0.0034 (16)0.0010 (19)0.0025 (17)
S2410.0427 (9)0.0401 (9)0.0215 (9)0.0036 (7)0.0094 (6)0.0130 (6)
C2410.020 (3)0.014 (2)0.017 (3)0.0011 (19)0.004 (2)0.003 (2)
N2410.024 (2)0.0084 (19)0.015 (3)0.0010 (16)0.0018 (18)0.0026 (16)
Co30.0125 (3)0.0090 (3)0.0128 (4)0.0003 (2)0.0007 (2)0.0023 (2)
N810.020 (2)0.018 (2)0.013 (2)0.0019 (17)0.0024 (17)0.0008 (17)
C810.018 (3)0.013 (2)0.025 (3)0.0009 (19)0.003 (2)0.002 (2)
C820.020 (3)0.022 (3)0.031 (3)0.007 (2)0.002 (2)0.000 (2)
C830.014 (3)0.022 (3)0.025 (3)0.000 (2)0.002 (2)0.009 (2)
C840.022 (3)0.015 (2)0.019 (3)0.004 (2)0.003 (2)0.004 (2)
C850.018 (3)0.017 (3)0.020 (3)0.002 (2)0.002 (2)0.005 (2)
C860.015 (3)0.017 (2)0.028 (3)0.003 (2)0.000 (2)0.000 (2)
C870.017 (3)0.023 (3)0.032 (3)0.007 (2)0.000 (2)0.006 (2)
C880.018 (3)0.017 (3)0.020 (3)0.001 (2)0.001 (2)0.000 (2)
C890.020 (3)0.016 (2)0.027 (3)0.008 (2)0.003 (2)0.002 (2)
C900.020 (3)0.015 (2)0.022 (3)0.003 (2)0.001 (2)0.008 (2)
C910.018 (3)0.015 (2)0.024 (3)0.003 (2)0.003 (2)0.000 (2)
C920.018 (3)0.020 (3)0.021 (3)0.002 (2)0.005 (2)0.005 (2)
N820.025 (2)0.0050 (19)0.013 (2)0.0008 (16)0.0027 (17)0.0011 (16)
N1010.015 (2)0.0127 (19)0.013 (2)0.0002 (15)0.0016 (16)0.0073 (17)
C1010.038 (3)0.012 (2)0.019 (3)0.002 (2)0.003 (2)0.002 (2)
C1020.055 (4)0.014 (3)0.019 (3)0.002 (2)0.009 (3)0.008 (2)
C1030.024 (3)0.012 (2)0.020 (3)0.0024 (19)0.004 (2)0.007 (2)
C1040.026 (3)0.013 (2)0.019 (3)0.000 (2)0.001 (2)0.000 (2)
C1050.024 (3)0.013 (2)0.013 (3)0.0021 (19)0.002 (2)0.002 (2)
C1060.044 (3)0.012 (3)0.020 (3)0.002 (2)0.004 (2)0.004 (2)
C1070.035 (3)0.016 (3)0.016 (3)0.003 (2)0.002 (2)0.002 (2)
C1080.021 (3)0.011 (2)0.022 (3)0.0008 (19)0.005 (2)0.001 (2)
C1090.034 (3)0.011 (2)0.023 (3)0.000 (2)0.003 (2)0.000 (2)
C1100.028 (3)0.021 (3)0.017 (3)0.004 (2)0.004 (2)0.005 (2)
C1110.032 (3)0.013 (2)0.018 (3)0.002 (2)0.002 (2)0.002 (2)
C1120.044 (3)0.013 (2)0.017 (3)0.003 (2)0.000 (2)0.007 (2)
N1020.013 (2)0.0136 (19)0.017 (2)0.0005 (15)0.0018 (16)0.0040 (17)
S2510.0628 (11)0.0365 (9)0.0205 (9)0.0032 (7)0.0086 (7)0.0028 (6)
C2510.025 (3)0.009 (2)0.022 (3)0.0019 (19)0.005 (2)0.004 (2)
N2510.024 (2)0.016 (2)0.020 (3)0.0006 (17)0.0048 (19)0.0053 (18)
S2610.0608 (10)0.0308 (8)0.0150 (8)0.0058 (7)0.0115 (7)0.0048 (6)
C2610.021 (3)0.010 (2)0.016 (3)0.0002 (19)0.002 (2)0.0026 (19)
N2610.021 (2)0.013 (2)0.016 (3)0.0014 (16)0.0009 (18)0.0032 (17)
N1210.052 (4)0.040 (3)0.043 (4)0.006 (3)0.006 (3)0.006 (3)
C1210.048 (4)0.042 (4)0.037 (4)0.007 (3)0.015 (3)0.007 (3)
C1220.038 (3)0.023 (3)0.032 (4)0.001 (2)0.006 (3)0.001 (3)
C1230.039 (3)0.022 (3)0.025 (3)0.001 (2)0.006 (3)0.001 (2)
C1240.031 (3)0.050 (4)0.056 (5)0.001 (3)0.002 (3)0.007 (3)
C1250.043 (4)0.046 (4)0.061 (5)0.007 (3)0.004 (3)0.018 (4)
C1260.031 (3)0.026 (3)0.028 (3)0.001 (2)0.008 (2)0.001 (2)
C1270.031 (3)0.026 (3)0.030 (4)0.001 (2)0.007 (3)0.002 (2)
C1280.030 (3)0.026 (3)0.034 (4)0.007 (2)0.004 (3)0.000 (3)
C1290.034 (3)0.028 (3)0.025 (3)0.000 (2)0.001 (2)0.002 (2)
C1300.038 (4)0.029 (3)0.042 (4)0.006 (3)0.002 (3)0.004 (3)
C1310.040 (4)0.045 (4)0.052 (5)0.006 (3)0.005 (3)0.011 (3)
C1320.035 (3)0.038 (3)0.043 (4)0.008 (3)0.000 (3)0.001 (3)
N1220.044 (3)0.035 (3)0.043 (4)0.002 (2)0.000 (3)0.010 (2)
N1410.066 (4)0.046 (3)0.047 (4)0.010 (3)0.013 (3)0.013 (3)
C1410.055 (4)0.038 (4)0.045 (5)0.017 (3)0.016 (3)0.006 (3)
C1420.045 (4)0.037 (3)0.038 (4)0.010 (3)0.013 (3)0.003 (3)
C1430.043 (4)0.022 (3)0.030 (4)0.001 (2)0.009 (3)0.002 (3)
C1440.044 (4)0.045 (4)0.048 (5)0.004 (3)0.011 (3)0.007 (3)
C1450.052 (4)0.046 (4)0.068 (6)0.003 (3)0.010 (4)0.014 (4)
C1460.040 (3)0.028 (3)0.033 (4)0.013 (3)0.011 (3)0.002 (3)
C1470.039 (3)0.019 (3)0.031 (4)0.007 (2)0.008 (3)0.002 (2)
C1480.039 (3)0.027 (3)0.029 (4)0.010 (2)0.006 (3)0.007 (3)
C1490.039 (4)0.038 (4)0.044 (4)0.011 (3)0.002 (3)0.011 (3)
C1500.032 (4)0.061 (5)0.067 (6)0.011 (3)0.001 (3)0.025 (4)
C1510.035 (4)0.041 (4)0.056 (5)0.009 (3)0.004 (3)0.010 (3)
C1520.034 (3)0.049 (4)0.039 (4)0.005 (3)0.001 (3)0.000 (3)
N1420.043 (3)0.042 (3)0.046 (4)0.011 (2)0.001 (3)0.008 (3)
N1610.052 (4)0.043 (3)0.040 (4)0.000 (3)0.001 (3)0.004 (3)
C1610.046 (4)0.039 (4)0.050 (5)0.009 (3)0.010 (3)0.005 (3)
C1620.035 (3)0.033 (3)0.037 (4)0.000 (3)0.004 (3)0.006 (3)
C1630.036 (3)0.019 (3)0.030 (4)0.001 (2)0.002 (3)0.005 (2)
C1640.033 (4)0.045 (4)0.058 (5)0.003 (3)0.003 (3)0.009 (3)
C1650.039 (4)0.052 (4)0.073 (6)0.006 (3)0.007 (4)0.006 (4)
C1660.032 (3)0.023 (3)0.035 (4)0.004 (2)0.007 (2)0.005 (2)
N1710.048 (3)0.036 (3)0.044 (4)0.004 (2)0.004 (3)0.010 (3)
C1710.042 (4)0.037 (4)0.048 (5)0.011 (3)0.004 (3)0.009 (3)
C1720.036 (3)0.034 (3)0.040 (4)0.003 (3)0.006 (3)0.001 (3)
C1730.039 (3)0.019 (3)0.034 (4)0.001 (2)0.008 (3)0.000 (2)
C1740.033 (4)0.049 (4)0.050 (5)0.005 (3)0.005 (3)0.019 (3)
C1750.034 (4)0.036 (4)0.070 (5)0.002 (3)0.001 (3)0.019 (3)
C1760.036 (3)0.025 (3)0.034 (4)0.005 (2)0.006 (3)0.001 (3)
Geometric parameters (Å, º) top
Co1—N2112.063 (4)N81—C811.348 (6)
Co1—N2212.063 (4)C81—C821.378 (7)
Co1—N22i2.196 (4)C81—H810.9500
Co1—N212.216 (4)C82—C831.413 (7)
Co1—N2ii2.216 (4)C82—H820.9500
Co1—N12.245 (3)C83—C841.393 (7)
N1—C11.333 (6)C83—C861.463 (7)
N1—C51.350 (6)C84—C851.378 (7)
C1—C21.394 (7)C84—H840.9500
C1—H10.9500C85—H850.9500
C2—C31.383 (7)C86—C871.336 (7)
C2—H20.9500C86—H860.9500
C3—C41.397 (7)C87—C881.475 (7)
C3—C61.481 (6)C87—H870.9500
C4—C51.380 (7)C88—C891.364 (7)
C4—H40.9500C88—C921.410 (7)
C5—H50.9500C89—C901.383 (7)
C6—C71.299 (7)C89—H890.9500
C6—H60.9500C90—N821.363 (6)
C7—C81.481 (6)C90—H900.9500
C7—H70.9500C91—N821.351 (6)
C8—C121.386 (7)C91—C921.377 (7)
C8—C91.394 (7)C91—H910.9500
C9—C101.390 (6)C92—H920.9500
C9—H90.9500N82—Co3i2.167 (4)
C10—N21.348 (6)N101—C1051.338 (6)
C10—H100.9500N101—C1011.339 (6)
C11—N21.340 (6)C101—C1021.376 (7)
C11—C121.388 (6)C101—H1010.9500
C11—H110.9500C102—C1031.392 (7)
C12—H120.9500C102—H1020.9500
N2—Co1iii2.216 (4)C103—C1041.394 (7)
N21—C251.335 (6)C103—C1061.466 (7)
N21—C211.359 (6)C104—C1051.385 (7)
C21—C221.386 (7)C104—H1040.9500
C21—H210.9500C105—H1050.9500
C22—C231.391 (7)C106—C1071.325 (7)
C22—H220.9500C106—H1060.9500
C23—C241.415 (7)C107—C1081.458 (7)
C23—C261.469 (7)C107—H1070.9500
C24—C251.374 (7)C108—C1091.385 (7)
C24—H240.9500C108—C1121.393 (7)
C25—H250.9500C109—C1101.380 (7)
C26—C271.353 (7)C109—H1090.9500
C26—H260.9500C110—N1021.342 (6)
C27—C281.460 (7)C110—H1100.9500
C27—H270.9500C111—N1021.346 (6)
C28—C321.379 (7)C111—C1121.378 (7)
C28—C291.415 (7)C111—H1110.9500
C29—C301.383 (7)C112—H1120.9500
C29—H290.9500N102—Co3iii2.233 (4)
C30—N221.307 (7)S251—C2511.624 (6)
C30—H300.9500C251—N2511.170 (7)
C31—N221.360 (7)S261—C2611.623 (5)
C31—C321.375 (7)C261—N2611.160 (6)
C31—H310.9500N121—C1211.328 (9)
C32—H320.9500N121—C1251.336 (9)
N22—Co1iv2.196 (4)C121—C1221.383 (9)
S211—C2111.625 (6)C121—H1210.9500
C211—N2111.179 (6)C122—C1231.400 (8)
S221—C2211.619 (5)C122—H1220.9500
C221—N2211.175 (6)C123—C1241.387 (9)
Co2—N2412.075 (4)C123—C1261.475 (8)
Co2—N2312.077 (4)C124—C1251.373 (9)
Co2—N612.167 (4)C124—H1240.9500
Co2—N62i2.222 (4)C125—H1250.9500
Co2—N412.223 (4)C126—C1271.325 (8)
Co2—N42iii2.231 (4)C126—H1260.9500
N41—C411.338 (6)C127—C1281.473 (8)
N41—C451.347 (6)C127—H1270.9500
C41—C421.378 (7)C128—C1321.383 (9)
C41—H410.9500C128—C1291.393 (8)
C42—C431.389 (7)C129—C1301.380 (8)
C42—H420.9500C129—H1290.9500
C43—C441.381 (7)C130—N1221.334 (8)
C43—C461.473 (6)C130—H1300.9500
C44—C451.382 (7)C131—N1221.335 (8)
C44—H440.9500C131—C1321.375 (9)
C45—H450.9500C131—H1310.9500
C46—C471.314 (7)C132—H1320.9500
C46—H460.9500N141—C1451.324 (9)
C47—C481.454 (6)N141—C1411.363 (9)
C47—H470.9500C141—C1421.367 (9)
C48—C491.387 (7)C141—H1410.9500
C48—C521.400 (7)C142—C1431.386 (8)
C49—C501.387 (6)C142—H1420.9500
C49—H490.9500C143—C1441.395 (9)
C50—N421.342 (6)C143—C1461.466 (8)
C50—H500.9500C144—C1451.378 (10)
C51—N421.337 (6)C144—H1440.9500
C51—C521.383 (7)C145—H1450.9500
C51—H510.9500C146—C1471.318 (9)
C52—H520.9500C146—H1460.9500
N42—Co2ii2.231 (4)C147—C1481.470 (8)
N61—C611.334 (6)C147—H1470.9500
N61—C651.363 (6)C148—C1491.399 (9)
C61—C621.374 (7)C148—C1521.404 (8)
C61—H610.9500C149—C1501.377 (9)
C62—C631.397 (7)C149—H1490.9500
C62—H620.9500C150—N1421.334 (8)
C63—C641.395 (8)C150—H1500.9500
C63—C661.473 (7)C151—C1521.347 (9)
C64—C651.382 (7)C151—N1421.360 (8)
C64—H640.9500C151—H1510.9500
C65—H650.9500C152—H1520.9500
C66—C671.344 (7)N161—C1651.336 (9)
C66—H660.9500N161—C1611.345 (9)
C67—C681.474 (7)C161—C1621.370 (9)
C67—H670.9500C161—H1610.9500
C68—C721.370 (7)C162—C1631.380 (8)
C68—C691.414 (7)C162—H1620.9500
C69—C701.368 (7)C163—C1641.385 (9)
C69—H690.9500C163—C1661.472 (8)
C70—N621.347 (6)C164—C1651.374 (10)
C70—H700.9500C164—H1640.9500
C71—N621.351 (6)C165—H1650.9500
C71—C721.376 (7)C166—C166v1.340 (11)
C71—H710.9500C166—H1660.9500
C72—H720.9500N171—C1751.327 (8)
N62—Co2iv2.222 (4)N171—C1711.338 (8)
S231—C2311.635 (5)C171—C1721.362 (9)
C231—N2311.162 (6)C171—H1710.9500
S241—C2411.627 (5)C172—C1731.398 (8)
C241—N2411.176 (6)C172—H1720.9500
Co3—N2512.051 (5)C173—C1741.384 (9)
Co3—N2612.071 (4)C173—C1761.476 (8)
Co3—N82iv2.167 (4)C174—C1751.391 (9)
Co3—N812.223 (4)C174—H1740.9500
Co3—N1012.228 (4)C175—H1750.9500
Co3—N102ii2.233 (4)C176—C176vi1.311 (12)
N81—C851.338 (6)C176—H1760.9500
N211—Co1—N221178.91 (15)N251—Co3—N10190.66 (15)
N211—Co1—N22i89.41 (17)N261—Co3—N10189.11 (15)
N221—Co1—N22i90.09 (17)N82iv—Co3—N10188.05 (14)
N211—Co1—N2191.99 (15)N81—Co3—N10191.90 (14)
N221—Co1—N2188.55 (15)N251—Co3—N102ii88.42 (15)
N22i—Co1—N21177.48 (16)N261—Co3—N102ii91.90 (15)
N211—Co1—N2ii90.75 (15)N82iv—Co3—N102ii87.70 (14)
N221—Co1—N2ii90.18 (14)N81—Co3—N102ii92.39 (14)
N22i—Co1—N2ii86.22 (16)N101—Co3—N102ii175.64 (14)
N21—Co1—N2ii91.67 (14)C85—N81—C81116.5 (4)
N211—Co1—N190.22 (15)C85—N81—Co3122.7 (3)
N221—Co1—N188.82 (14)C81—N81—Co3120.8 (3)
N22i—Co1—N191.59 (16)N81—C81—C82123.4 (4)
N21—Co1—N190.49 (13)N81—C81—H81118.3
N2ii—Co1—N1177.59 (14)C82—C81—H81118.3
C1—N1—C5116.7 (4)C81—C82—C83120.1 (4)
C1—N1—Co1122.3 (3)C81—C82—H82119.9
C5—N1—Co1120.9 (3)C83—C82—H82119.9
N1—C1—C2124.0 (5)C84—C83—C82115.6 (4)
N1—C1—H1118.0C84—C83—C86124.6 (4)
C2—C1—H1118.0C82—C83—C86119.7 (4)
C3—C2—C1119.2 (4)C85—C84—C83120.4 (4)
C3—C2—H2120.4C85—C84—H84119.8
C1—C2—H2120.4C83—C84—H84119.8
C2—C3—C4117.0 (4)N81—C85—C84123.9 (4)
C2—C3—C6124.4 (4)N81—C85—H85118.1
C4—C3—C6118.6 (4)C84—C85—H85118.1
C5—C4—C3120.2 (5)C87—C86—C83123.3 (5)
C5—C4—H4119.9C87—C86—H86118.3
C3—C4—H4119.9C83—C86—H86118.3
N1—C5—C4122.8 (4)C86—C87—C88125.6 (5)
N1—C5—H5118.6C86—C87—H87117.2
C4—C5—H5118.6C88—C87—H87117.2
C7—C6—C3125.3 (5)C89—C88—C92118.1 (4)
C7—C6—H6117.4C89—C88—C87119.9 (5)
C3—C6—H6117.4C92—C88—C87122.0 (5)
C6—C7—C8126.2 (5)C88—C89—C90120.1 (5)
C6—C7—H7116.9C88—C89—H89120.0
C8—C7—H7116.9C90—C89—H89120.0
C12—C8—C9117.5 (4)N82—C90—C89123.4 (4)
C12—C8—C7118.9 (5)N82—C90—H90118.3
C9—C8—C7123.7 (4)C89—C90—H90118.3
C10—C9—C8118.6 (5)N82—C91—C92124.5 (5)
C10—C9—H9120.7N82—C91—H91117.8
C8—C9—H9120.7C92—C91—H91117.8
N2—C10—C9124.4 (5)C91—C92—C88118.4 (5)
N2—C10—H10117.8C91—C92—H92120.8
C9—C10—H10117.8C88—C92—H92120.8
N2—C11—C12123.6 (4)C91—N82—C90115.5 (4)
N2—C11—H11118.2C91—N82—Co3i123.4 (3)
C12—C11—H11118.2C90—N82—Co3i120.9 (3)
C8—C12—C11119.8 (5)C105—N101—C101116.7 (4)
C8—C12—H12120.1C105—N101—Co3122.4 (3)
C11—C12—H12120.1C101—N101—Co3120.8 (3)
C11—N2—C10116.0 (4)N101—C101—C102123.0 (5)
C11—N2—Co1iii120.9 (3)N101—C101—H101118.5
C10—N2—Co1iii123.0 (3)C102—C101—H101118.5
C25—N21—C21115.1 (4)C101—C102—C103120.9 (5)
C25—N21—Co1122.4 (3)C101—C102—H102119.6
C21—N21—Co1122.4 (3)C103—C102—H102119.6
N21—C21—C22124.9 (4)C102—C103—C104116.0 (4)
N21—C21—H21117.5C102—C103—C106120.2 (5)
C22—C21—H21117.5C104—C103—C106123.8 (5)
C21—C22—C23119.1 (4)C105—C104—C103119.6 (5)
C21—C22—H22120.4C105—C104—H104120.2
C23—C22—H22120.4C103—C104—H104120.2
C22—C23—C24116.2 (4)N101—C105—C104123.8 (5)
C22—C23—C26124.7 (4)N101—C105—H105118.1
C24—C23—C26119.0 (4)C104—C105—H105118.1
C25—C24—C23120.1 (4)C107—C106—C103126.7 (5)
C25—C24—H24119.9C107—C106—H106116.7
C23—C24—H24119.9C103—C106—H106116.7
N21—C25—C24124.5 (4)C106—C107—C108126.0 (5)
N21—C25—H25117.8C106—C107—H107117.0
C24—C25—H25117.8C108—C107—H107117.0
C27—C26—C23122.6 (4)C109—C108—C112115.7 (4)
C27—C26—H26118.7C109—C108—C107125.4 (5)
C23—C26—H26118.7C112—C108—C107118.9 (5)
C26—C27—C28122.7 (5)C110—C109—C108120.6 (5)
C26—C27—H27118.7C110—C109—H109119.7
C28—C27—H27118.7C108—C109—H109119.7
C32—C28—C29117.1 (5)N102—C110—C109123.5 (5)
C32—C28—C27124.6 (5)N102—C110—H110118.2
C29—C28—C27118.3 (4)C109—C110—H110118.2
C30—C29—C28118.7 (5)N102—C111—C112123.0 (5)
C30—C29—H29120.6N102—C111—H111118.5
C28—C29—H29120.6C112—C111—H111118.5
N22—C30—C29124.2 (5)C111—C112—C108120.9 (5)
N22—C30—H30117.9C111—C112—H112119.6
C29—C30—H30117.9C108—C112—H112119.6
N22—C31—C32123.1 (5)C110—N102—C111116.3 (4)
N22—C31—H31118.4C110—N102—Co3iii123.0 (3)
C32—C31—H31118.4C111—N102—Co3iii120.7 (3)
C31—C32—C28119.6 (5)N251—C251—S251179.2 (5)
C31—C32—H32120.2C251—N251—Co3162.1 (4)
C28—C32—H32120.2N261—C261—S261178.5 (4)
C30—N22—C31117.1 (4)C261—N261—Co3155.5 (4)
C30—N22—Co1iv121.9 (4)C121—N121—C125115.0 (6)
C31—N22—Co1iv120.9 (3)N121—C121—C122124.6 (6)
N211—C211—S211178.7 (5)N121—C121—H121117.7
C211—N211—Co1161.2 (4)C122—C121—H121117.7
N221—C221—S221179.0 (5)C121—C122—C123119.7 (6)
C221—N221—Co1158.5 (4)C121—C122—H122120.1
N241—Co2—N231178.11 (15)C123—C122—H122120.1
N241—Co2—N6189.14 (16)C124—C123—C122115.5 (6)
N231—Co2—N6189.11 (16)C124—C123—C126120.2 (5)
N241—Co2—N62i89.70 (16)C122—C123—C126124.3 (5)
N231—Co2—N62i92.07 (16)C125—C124—C123120.1 (6)
N61—Co2—N62i178.36 (15)C125—C124—H124119.9
N241—Co2—N4189.74 (14)C123—C124—H124119.9
N231—Co2—N4190.91 (14)N121—C125—C124124.9 (6)
N61—Co2—N4188.28 (14)N121—C125—H125117.5
N62i—Co2—N4190.57 (14)C124—C125—H125117.5
N241—Co2—N42iii89.30 (14)C127—C126—C123126.6 (5)
N231—Co2—N42iii89.98 (14)C127—C126—H126116.7
N61—Co2—N42iii89.52 (14)C123—C126—H126116.7
N62i—Co2—N42iii91.62 (14)C126—C127—C128126.2 (5)
N41—Co2—N42iii177.61 (14)C126—C127—H127116.9
C41—N41—C45116.1 (4)C128—C127—H127116.9
C41—N41—Co2120.1 (3)C132—C128—C129116.0 (6)
C45—N41—Co2123.8 (3)C132—C128—C127120.8 (5)
N41—C41—C42123.6 (5)C129—C128—C127123.2 (5)
N41—C41—H41118.2C130—C129—C128119.2 (6)
C42—C41—H41118.2C130—C129—H129120.4
C41—C42—C43120.3 (5)C128—C129—H129120.4
C41—C42—H42119.9N122—C130—C129125.1 (6)
C43—C42—H42119.9N122—C130—H130117.5
C44—C43—C42116.5 (4)C129—C130—H130117.5
C44—C43—C46124.7 (4)N122—C131—C132124.1 (6)
C42—C43—C46118.9 (4)N122—C131—H131118.0
C43—C44—C45120.1 (5)C132—C131—H131118.0
C43—C44—H44120.0C131—C132—C128120.6 (6)
C45—C44—H44120.0C131—C132—H132119.7
N41—C45—C44123.5 (5)C128—C132—H132119.7
N41—C45—H45118.2C130—N122—C131115.0 (5)
C44—C45—H45118.2C145—N141—C141115.2 (6)
C47—C46—C43126.5 (5)N141—C141—C142124.5 (6)
C47—C46—H46116.8N141—C141—H141117.8
C43—C46—H46116.8C142—C141—H141117.8
C46—C47—C48125.9 (5)C141—C142—C143120.0 (7)
C46—C47—H47117.0C141—C142—H142120.0
C48—C47—H47117.0C143—C142—H142120.0
C49—C48—C52115.7 (4)C142—C143—C144115.7 (6)
C49—C48—C47124.9 (4)C142—C143—C146124.3 (6)
C52—C48—C47119.4 (4)C144—C143—C146120.0 (5)
C50—C49—C48120.6 (4)C145—C144—C143120.8 (6)
C50—C49—H49119.7C145—C144—H144119.6
C48—C49—H49119.7C143—C144—H144119.6
N42—C50—C49123.5 (5)N141—C145—C144123.9 (7)
N42—C50—H50118.2N141—C145—H145118.0
C49—C50—H50118.2C144—C145—H145118.0
N42—C51—C52123.9 (5)C147—C146—C143126.4 (5)
N42—C51—H51118.0C147—C146—H146116.8
C52—C51—H51118.0C143—C146—H146116.8
C51—C52—C48120.1 (5)C146—C147—C148125.8 (5)
C51—C52—H52119.9C146—C147—H147117.1
C48—C52—H52119.9C148—C147—H147117.1
C51—N42—C50116.1 (4)C149—C148—C152115.2 (6)
C51—N42—Co2ii120.1 (3)C149—C148—C147121.2 (5)
C50—N42—Co2ii123.8 (3)C152—C148—C147123.5 (6)
C61—N61—C65115.7 (4)C150—C149—C148120.7 (6)
C61—N61—Co2121.5 (3)C150—C149—H149119.7
C65—N61—Co2122.8 (3)C148—C149—H149119.7
N61—C61—C62124.6 (5)N142—C150—C149124.1 (6)
N61—C61—H61117.7N142—C150—H150118.0
C62—C61—H61117.7C149—C150—H150118.0
C61—C62—C63119.4 (5)C152—C151—N142125.5 (6)
C61—C62—H62120.3C152—C151—H151117.2
C63—C62—H62120.3N142—C151—H151117.2
C64—C63—C62117.4 (4)C151—C152—C148119.9 (6)
C64—C63—C66124.2 (5)C151—C152—H152120.1
C62—C63—C66118.4 (5)C148—C152—H152120.1
C65—C64—C63118.9 (5)C150—N142—C151114.6 (6)
C65—C64—H64120.5C165—N161—C161114.5 (6)
C63—C64—H64120.5N161—C161—C162124.2 (6)
N61—C65—C64124.0 (5)N161—C161—H161117.9
N61—C65—H65118.0C162—C161—H161117.9
C64—C65—H65118.0C161—C162—C163120.9 (6)
C67—C66—C63123.0 (5)C161—C162—H162119.6
C67—C66—H66118.5C163—C162—H162119.6
C63—C66—H66118.5C162—C163—C164115.5 (6)
C66—C67—C68122.4 (5)C162—C163—C166124.6 (5)
C66—C67—H67118.8C164—C163—C166119.9 (5)
C68—C67—H67118.8C165—C164—C163120.1 (6)
C72—C68—C69115.5 (5)C165—C164—H164119.9
C72—C68—C67120.7 (5)C163—C164—H164119.9
C69—C68—C67123.7 (5)N161—C165—C164124.9 (6)
C70—C69—C68120.0 (5)N161—C165—H165117.6
C70—C69—H69120.0C164—C165—H165117.6
C68—C69—H69120.0C166v—C166—C163125.5 (7)
N62—C70—C69124.1 (4)C166v—C166—H166117.3
N62—C70—H70118.0C163—C166—H166117.3
C69—C70—H70118.0C175—N171—C171115.5 (6)
N62—C71—C72123.3 (4)N171—C171—C172125.0 (6)
N62—C71—H71118.3N171—C171—H171117.5
C72—C71—H71118.3C172—C171—H171117.5
C68—C72—C71121.4 (5)C171—C172—C173119.9 (6)
C68—C72—H72119.3C171—C172—H172120.1
C71—C72—H72119.3C173—C172—H172120.1
C70—N62—C71115.6 (4)C174—C173—C172115.5 (6)
C70—N62—Co2iv123.3 (3)C174—C173—C176119.9 (5)
C71—N62—Co2iv121.0 (3)C172—C173—C176124.5 (6)
N231—C231—S231179.3 (5)C173—C174—C175120.5 (6)
C231—N231—Co2156.4 (4)C173—C174—H174119.8
N241—C241—S241177.3 (4)C175—C174—H174119.8
C241—N241—Co2150.4 (4)N171—C175—C174123.6 (6)
N251—Co3—N261178.71 (16)N171—C175—H175118.2
N251—Co3—N82iv91.05 (16)C174—C175—H175118.2
N261—Co3—N82iv90.21 (16)C176vi—C176—C173126.2 (7)
N251—Co3—N8191.35 (16)C176vi—C176—H176116.9
N261—Co3—N8187.39 (15)C173—C176—H176116.9
N82iv—Co3—N81177.60 (16)
Symmetry codes: (i) x+1, y, z; (ii) x, y1, z; (iii) x, y+1, z; (iv) x1, y, z; (v) x+1, y+2, z+1; (vi) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Co(NCS)2(C12H10N2)2]·C12H10N2
Mr721.75
Crystal system, space groupTriclinic, P1
Temperature (K)170
a, b, c (Å)13.7954 (14), 13.8916 (13), 27.848 (2)
α, β, γ (°)99.892 (10), 90.547 (11), 91.269 (11)
V3)5255.7 (8)
Z6
Radiation typeMo Kα
µ (mm1)0.65
Crystal size (mm)0.3 × 0.2 × 0.2
Data collection
DiffractometerStoe IPDS1
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
15899, 15899, 11067
Rint0.000
θmax (°)24.1
(sin θ/λ)max1)0.573
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.054, 0.166, 1.03
No. of reflections15899
No. of parameters1326
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.84, 0.68

Computer programs: X-AREA (Stoe & Cie, 2008), X-RED32 (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011), CIFTAB (Sheldrick, 2008).

 

Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. NA 720/3-1) and the State of Schleswig-Holstein. We thank Professor Dr Bensch for access to his experimental facility.

References

First citationBoeckmann, J. & Näther, C. (2010). Dalton Trans. 39, 1119–1126.  Web of Science CSD CrossRef
First citationBrandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany.
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals
First citationStoe & Cie (2008). X-AREA and X-RED32. Stoe & Cie, Darmstadt, Germany.
First citationWöhlert, S., Boeckmann, J., Wriedt, M. & Näther, C. (2011). Angew. Chem. Int. Ed., 50, 6920–6923.
First citationWriedt, M., Jess, I. & Näther, C. (2009). Eur. J. Inorg. Chem. pp. 1406–1413.  Web of Science CSD CrossRef

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Volume 68| Part 6| June 2012| Pages m733-m734
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