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

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COMMUNICATIONS
ISSN: 2056-9890

Tetra­kis(ethyl pyridine-4-carboxyl­ate-κN)bis­­(thio­cyanato-κN)cobalt(II)

aCollege of Chemistry and Chemical Engineering, Huaihua University, Huaihua 418008, People's Republic of China, and bWuling Electric Power Group Corporation, Changsha 410000, People's Republic of China
*Correspondence e-mail: xiulingfeng2001@sina.com

(Received 19 March 2012; accepted 15 May 2012; online 19 May 2012)

In the title complex, [Co(NCS)2(C8H9NO2)4], the CoII atom is six-coordinated by four N atoms from four ethyl pyridine-4-carboxyl­ate ligands in the equatorial plane and two N atoms of thio­cyanate ligands in the axial positions, showing a slightly distorted octa­hedral geometry. The structure exhibits disorder in one of the ethyl chains, which was refined using a two-site model with 0.70 (6):0.30 (6) occupancy.

Related literature

For the structures of related complexes containing ethyl pyridine-4-carboxyl­ate ligands, see: Wang et al. (2012[Wang, N., Sun, X., Wan, D., Chen, J. & Li, B. (2012). Acta Cryst. E68, m204-m205.]). For other related structures, see: Manna et al. (2008[Manna, S. C., Jana, A. D., Drew, M. G. B. & Mostafa, G. (2008). Polyhedron, 27, 1280-1286.]); Diehr et al. (2011[Diehr, S., Wöhlert, S., Boeckmann, J. & Näther, C. (2011). Acta Cryst. E67, m1898.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(NCS)2(C8H9NO2)4]

  • Mr = 779.74

  • Monoclinic, P 21

  • a = 11.2190 (11) Å

  • b = 14.3742 (16) Å

  • c = 12.0189 (13) Å

  • β = 96.430 (1)°

  • V = 1926.0 (4) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.61 mm−1

  • T = 298 K

  • 0.48 × 0.40 × 0.30 mm

Data collection
  • Bruker SMART 1000 CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2002[Bruker (2002). SAINT, SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.759, Tmax = 0.838

  • 10061 measured reflections

  • 5985 independent reflections

  • 4025 reflections with I > 2σ(I)

  • Rint = 0.037

Refinement
  • R[F2 > 2σ(F2)] = 0.047

  • wR(F2) = 0.122

  • S = 1.03

  • 5985 reflections

  • 484 parameters

  • 1 restraint

  • H-atom parameters constrained

  • Δρmax = 0.37 e Å−3

  • Δρmin = −0.28 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 2433 Friedel pairs

  • Flack parameter: −0.04 (2)

Data collection: SMART (Bruker, 2002[Bruker (2002). SAINT, SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2002[Bruker (2002). SAINT, SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

Coordination compounds with N-heterocyclic ligands have been extensively studied due to the diversity of their structures. Many coordination complexes with N-heterocyclic and thiocyanate ligands have been reported (Wang et al., 2012; Manna et al., 2008; Diehr et al., 2011). As part of our further studies on this class of compounds, we report here the crystal structure of the title compound.

In the title complex, Co(C8H9NO2)4(SCN)2, the CoII atom is six-coordinated with four N atoms from four ethyl pyridine-4-carboxylate ligands in the equatorial plane and two N atoms of thiocyanatos in the axial positions(Fig.1), showing a slightly distorted octahedral geometry. The equatorial Co—N distances are in the range of 2.192 (4) ~ 2.209 (4) Å which are significantly longer than the axial Co—N bond distances of 2.041 (5) and 2.071 (5) Å. The title complex exhibits a zero-dimensional structure.

Related literature top

For the structures of related complexes containing ethyl pyridine-4-carboxylate ligands, see: Wang et al. (2012). For other related structures, see: Manna et al. (2008); Diehr et al. (2011).

Experimental top

A mixture of CoCl2.6H2O (0.5 mmol), pyridine-4-carboxylic acid (2 mmol), 3-aminopropanoic acid (1 mmol) and KSCN (1 mmol) in a 40% aqueous solution of ethanol (15 mL) was heated at 413 K in a Teflon-lined stainless steel autoclave for three days. The reaction system was then slowly cooled to room temperature. Red crystals of the title compound suitable for single-crystal X-ray diffraction analysis were obtained by slow evaporation of aqua solution over a period of one month (yield 30% based on Co).

Refinement top

All H atoms attached to C atoms were fixed geometrically and treated as riding with C—H = 0.93 Å (CH), 0.97 Å (CH2) and 0.96 Å (CH3), and with Uiso(H) = 1.5Ueq(C) for the methyl group and Uiso(H) = 1.2Ueq(C) for all others. The two C atoms (C15 and C16) of an ethyl pyridine-4-carboxylate are disordered over two positions in a 0.70 (6):0.30 (6) ratio.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms have been omitted for clarity. Both disorder models are shown.
Tetrakis(ethyl pyridine-4-carboxylate-κN)bis(thiocyanato-κN)cobalt(II) top
Crystal data top
[Co(NCS)2(C8H9NO2)4]F(000) = 810
Mr = 779.74Dx = 1.345 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 2899 reflections
a = 11.2190 (11) Åθ = 2.3–21.7°
b = 14.3742 (16) ŵ = 0.61 mm1
c = 12.0189 (13) ÅT = 298 K
β = 96.430 (1)°Block, red
V = 1926.0 (4) Å30.48 × 0.40 × 0.30 mm
Z = 2
Data collection top
Bruker SMART 1000 CCD
diffractometer
5985 independent reflections
Radiation source: fine-focus sealed tube4025 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
phi and ω scansθmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1313
Tmin = 0.759, Tmax = 0.838k = 1716
10061 measured reflectionsl = 1413
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)] = 0.047H-atom parameters constrained
wR(F2) = 0.122 w = 1/[σ2(Fo2) + (0.0362P)2 + 0.8634P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
5985 reflectionsΔρmax = 0.37 e Å3
484 parametersΔρmin = 0.28 e Å3
1 restraintAbsolute structure: Flack (1983), 2433 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.04 (2)
Crystal data top
[Co(NCS)2(C8H9NO2)4]V = 1926.0 (4) Å3
Mr = 779.74Z = 2
Monoclinic, P21Mo Kα radiation
a = 11.2190 (11) ŵ = 0.61 mm1
b = 14.3742 (16) ÅT = 298 K
c = 12.0189 (13) Å0.48 × 0.40 × 0.30 mm
β = 96.430 (1)°
Data collection top
Bruker SMART 1000 CCD
diffractometer
5985 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
4025 reflections with I > 2σ(I)
Tmin = 0.759, Tmax = 0.838Rint = 0.037
10061 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.047H-atom parameters constrained
wR(F2) = 0.122Δρmax = 0.37 e Å3
S = 1.03Δρmin = 0.28 e Å3
5985 reflectionsAbsolute structure: Flack (1983), 2433 Friedel pairs
484 parametersAbsolute structure parameter: 0.04 (2)
1 restraint
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.41695 (6)0.42870 (5)0.29066 (6)0.0488 (2)
S10.5628 (2)0.74028 (15)0.3384 (2)0.1067 (8)
S20.2556 (2)0.12627 (16)0.2389 (3)0.1262 (9)
N10.4685 (4)0.3954 (3)0.1232 (4)0.0513 (12)
N20.5961 (4)0.3757 (3)0.3506 (4)0.0532 (12)
N30.3800 (4)0.4617 (3)0.4615 (4)0.0532 (12)
N40.2373 (4)0.4792 (3)0.2233 (4)0.0497 (11)
N50.4864 (4)0.5617 (4)0.2819 (4)0.0579 (12)
N60.3460 (4)0.2991 (4)0.3050 (4)0.0549 (12)
O10.6918 (3)0.4031 (3)0.2104 (3)0.0649 (11)
O20.7291 (4)0.2603 (3)0.1435 (4)0.0874 (14)
O30.9606 (5)0.2026 (6)0.4967 (6)0.131 (3)
O41.0350 (5)0.3214 (6)0.4168 (7)0.168 (3)
O50.1750 (4)0.5513 (4)0.7882 (4)0.0924 (15)
O60.3614 (4)0.5993 (4)0.8411 (4)0.0932 (16)
O70.1268 (4)0.6682 (4)0.1195 (4)0.0735 (13)
O80.1984 (4)0.5241 (4)0.0914 (5)0.1110 (19)
C10.4928 (5)0.4607 (4)0.0515 (5)0.0521 (14)
H10.46490.52060.06200.063*
C20.5579 (4)0.4448 (4)0.0386 (4)0.0516 (14)
H20.57240.49270.08730.062*
C30.6001 (5)0.3566 (4)0.0539 (4)0.0485 (13)
C40.5708 (5)0.2873 (4)0.0171 (5)0.0566 (15)
H40.59420.22620.00640.068*
C50.5065 (5)0.3098 (4)0.1042 (5)0.0558 (14)
H50.48850.26250.15250.067*
C60.6784 (5)0.3337 (5)0.1399 (5)0.0598 (15)
C70.7686 (6)0.3856 (5)0.2978 (6)0.086 (2)
H7A0.74660.42750.36000.103*
H7B0.75610.32250.32500.103*
C80.8956 (7)0.3986 (6)0.2577 (7)0.117 (3)
H8A0.90810.46080.22960.176*
H8B0.94310.38870.31830.176*
H8C0.91880.35490.19890.176*
C90.6916 (5)0.4149 (5)0.3136 (5)0.0694 (17)
H90.68040.46590.26600.083*
C100.8057 (6)0.3830 (5)0.3430 (6)0.084 (2)
H100.87070.41330.31740.101*
C110.8235 (5)0.3071 (5)0.4097 (6)0.0703 (18)
C120.7267 (6)0.2636 (5)0.4472 (5)0.0688 (17)
H120.73650.21100.49240.083*
C130.6137 (5)0.3007 (5)0.4153 (5)0.0607 (15)
H130.54740.27190.44030.073*
C140.9529 (8)0.2781 (8)0.4441 (8)0.101 (3)
C151.087 (2)0.186 (2)0.546 (3)0.130 (9)0.70 (6)
H15A1.09610.19920.62580.157*0.70 (6)
H15B1.14210.22390.50990.157*0.70 (6)
C161.108 (3)0.084 (3)0.526 (3)0.166 (12)0.70 (6)
H16A1.06040.04700.57060.249*0.70 (6)
H16B1.19140.06970.54540.249*0.70 (6)
H16C1.08610.06990.44800.249*0.70 (6)
C15'1.056 (5)0.136 (5)0.483 (7)0.12 (2)0.30 (6)
H15C1.08540.14550.41090.149*0.30 (6)
H15D1.02560.07330.48570.149*0.30 (6)
C16'1.158 (6)0.150 (5)0.576 (5)0.14 (2)0.30 (6)
H16D1.13950.20190.62190.212*0.30 (6)
H16E1.23080.16280.54400.212*0.30 (6)
H16F1.16740.09510.62110.212*0.30 (6)
C170.2728 (5)0.4426 (5)0.4944 (4)0.0608 (15)
H170.21860.40740.44760.073*
C180.2393 (5)0.4734 (4)0.5958 (5)0.0634 (17)
H180.16320.46070.61570.076*
C190.3204 (5)0.5229 (4)0.6662 (4)0.0590 (15)
C200.4324 (5)0.5384 (4)0.6346 (5)0.0609 (16)
H200.49020.56940.68240.073*
C210.4582 (5)0.5081 (4)0.5332 (5)0.0605 (16)
H210.53410.52020.51250.073*
C220.2895 (6)0.5621 (5)0.7750 (5)0.0677 (16)
C230.1327 (8)0.5898 (6)0.8912 (6)0.101 (3)
H23A0.06540.55330.91080.121*
H23B0.19650.58550.95250.121*
C240.0957 (9)0.6875 (8)0.8753 (7)0.121 (3)
H24A0.16410.72470.86290.182*
H24B0.06290.70930.94100.182*
H24C0.03610.69230.81180.182*
C250.1515 (5)0.4226 (5)0.1774 (4)0.0635 (14)
H250.17000.36000.16990.076*
C260.0371 (5)0.4514 (4)0.1404 (5)0.0652 (17)
H260.01930.40930.10780.078*
C270.0068 (5)0.5447 (4)0.1526 (5)0.0515 (14)
C280.0947 (5)0.6025 (4)0.1971 (5)0.0624 (16)
H280.07930.66570.20420.075*
C290.2082 (5)0.5672 (4)0.2323 (5)0.0607 (15)
H290.26660.60820.26380.073*
C300.1169 (6)0.5775 (6)0.1176 (5)0.0671 (18)
C310.2449 (6)0.7085 (6)0.0900 (6)0.087 (2)
H31A0.30190.68280.13660.104*
H31B0.27310.69570.01220.104*
C320.2313 (6)0.8104 (6)0.1087 (7)0.105 (3)
H32A0.20910.82220.18690.157*
H32B0.30590.84090.08490.157*
H32C0.17010.83390.06650.157*
C330.5190 (5)0.6359 (5)0.3058 (5)0.0550 (14)
C340.3064 (5)0.2267 (5)0.2801 (5)0.0580 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0440 (4)0.0428 (4)0.0603 (4)0.0030 (4)0.0096 (3)0.0021 (4)
S10.1289 (18)0.0693 (14)0.1272 (18)0.0407 (13)0.0373 (14)0.0361 (13)
S20.1069 (17)0.0605 (13)0.208 (3)0.0263 (13)0.0041 (17)0.0220 (16)
N10.048 (3)0.046 (3)0.061 (3)0.002 (2)0.009 (2)0.001 (2)
N20.046 (3)0.050 (3)0.064 (3)0.005 (2)0.010 (2)0.001 (2)
N30.047 (3)0.051 (3)0.062 (3)0.006 (2)0.005 (2)0.004 (2)
N40.049 (3)0.040 (3)0.061 (3)0.001 (2)0.010 (2)0.002 (2)
N50.055 (3)0.047 (3)0.073 (3)0.007 (3)0.013 (2)0.000 (3)
N60.051 (3)0.048 (3)0.066 (3)0.000 (3)0.007 (2)0.001 (3)
O10.078 (3)0.057 (3)0.064 (2)0.005 (2)0.0280 (19)0.001 (2)
O20.108 (4)0.062 (3)0.100 (4)0.026 (3)0.045 (3)0.006 (3)
O30.081 (4)0.138 (6)0.169 (7)0.042 (4)0.005 (4)0.028 (5)
O40.060 (4)0.196 (8)0.246 (8)0.006 (4)0.006 (4)0.077 (7)
O50.097 (4)0.118 (4)0.068 (3)0.019 (3)0.031 (3)0.024 (3)
O60.096 (4)0.101 (4)0.080 (3)0.010 (3)0.002 (3)0.036 (3)
O70.048 (3)0.072 (3)0.099 (4)0.014 (2)0.001 (2)0.007 (3)
O80.059 (3)0.106 (4)0.160 (5)0.019 (3)0.022 (3)0.014 (4)
C10.054 (3)0.038 (3)0.063 (4)0.006 (3)0.002 (3)0.004 (3)
C20.054 (3)0.049 (4)0.052 (3)0.006 (3)0.007 (2)0.001 (3)
C30.052 (3)0.044 (3)0.050 (3)0.007 (3)0.007 (3)0.001 (3)
C40.066 (4)0.040 (3)0.065 (4)0.008 (3)0.015 (3)0.003 (3)
C50.060 (3)0.046 (4)0.064 (4)0.001 (3)0.013 (3)0.005 (3)
C60.065 (4)0.049 (4)0.067 (4)0.011 (3)0.014 (3)0.005 (3)
C70.102 (5)0.084 (5)0.080 (4)0.003 (4)0.041 (4)0.006 (4)
C80.095 (6)0.111 (8)0.157 (7)0.007 (5)0.062 (5)0.001 (6)
C90.048 (3)0.074 (5)0.089 (4)0.004 (4)0.015 (3)0.010 (4)
C100.052 (4)0.087 (5)0.115 (6)0.003 (4)0.015 (4)0.012 (5)
C110.044 (4)0.080 (5)0.086 (5)0.008 (4)0.003 (3)0.011 (4)
C120.067 (4)0.063 (4)0.075 (4)0.005 (3)0.000 (3)0.002 (3)
C130.051 (4)0.060 (4)0.072 (4)0.007 (3)0.011 (3)0.004 (3)
C140.068 (6)0.110 (8)0.125 (7)0.014 (5)0.012 (5)0.027 (6)
C150.084 (13)0.14 (2)0.160 (19)0.025 (14)0.019 (14)0.007 (16)
C160.118 (19)0.15 (3)0.22 (2)0.044 (18)0.020 (18)0.01 (2)
C15'0.09 (3)0.13 (5)0.15 (4)0.03 (3)0.01 (3)0.01 (4)
C16'0.10 (4)0.13 (5)0.18 (4)0.01 (3)0.04 (3)0.03 (4)
C170.056 (3)0.068 (4)0.059 (3)0.016 (3)0.005 (2)0.011 (3)
C180.060 (4)0.076 (5)0.056 (4)0.013 (3)0.015 (3)0.008 (3)
C190.067 (4)0.058 (4)0.051 (3)0.001 (3)0.005 (3)0.007 (3)
C200.056 (4)0.066 (4)0.058 (4)0.009 (3)0.004 (3)0.010 (3)
C210.051 (3)0.068 (4)0.062 (4)0.007 (3)0.006 (3)0.006 (3)
C220.077 (5)0.064 (4)0.061 (4)0.000 (4)0.004 (4)0.009 (3)
C230.113 (6)0.119 (7)0.078 (5)0.014 (6)0.038 (5)0.018 (5)
C240.136 (9)0.137 (9)0.092 (7)0.025 (7)0.018 (6)0.016 (6)
C250.060 (3)0.049 (3)0.079 (4)0.001 (4)0.005 (3)0.004 (4)
C260.060 (4)0.057 (5)0.075 (4)0.014 (3)0.011 (3)0.003 (3)
C270.043 (3)0.053 (4)0.060 (3)0.001 (3)0.009 (3)0.009 (3)
C280.046 (3)0.049 (4)0.091 (4)0.001 (3)0.006 (3)0.004 (3)
C290.048 (3)0.049 (4)0.085 (4)0.006 (3)0.005 (3)0.001 (3)
C300.049 (4)0.073 (5)0.077 (4)0.002 (4)0.002 (3)0.011 (4)
C310.060 (4)0.101 (7)0.096 (5)0.022 (4)0.005 (4)0.000 (5)
C320.071 (5)0.107 (7)0.132 (7)0.024 (5)0.005 (4)0.012 (6)
C330.052 (3)0.052 (4)0.063 (4)0.006 (3)0.016 (3)0.000 (3)
C340.046 (3)0.052 (4)0.078 (4)0.000 (3)0.014 (3)0.009 (3)
Geometric parameters (Å, º) top
Co1—N62.041 (5)C10—H100.9300
Co1—N52.071 (5)C11—C121.372 (8)
Co1—N32.192 (4)C11—C141.523 (10)
Co1—N22.194 (5)C12—C131.390 (8)
Co1—N12.208 (4)C12—H120.9300
Co1—N42.209 (4)C13—H130.9300
S1—C331.614 (7)C15—C161.51 (7)
S2—C341.610 (7)C15—H15A0.9700
N1—C11.322 (6)C15—H15B0.9700
N1—C51.331 (6)C16—H16A0.9600
N2—C131.330 (7)C16—H16B0.9600
N2—C91.331 (7)C16—H16C0.9600
N3—C171.336 (6)C15'—C16'1.52 (14)
N3—C211.338 (6)C15'—H15C0.9700
N4—C291.314 (7)C15'—H15D0.9700
N4—C251.333 (7)C16'—H16D0.9600
N5—C331.153 (7)C16'—H16E0.9600
N6—C341.157 (7)C16'—H16F0.9600
O1—C61.329 (7)C17—C181.387 (7)
O1—C71.454 (7)C17—H170.9300
O2—C61.201 (7)C18—C191.370 (8)
O3—C141.254 (10)C18—H180.9300
O3—C15'1.46 (6)C19—C201.370 (8)
O3—C151.49 (3)C19—C221.500 (8)
O4—C141.188 (9)C20—C211.356 (7)
O5—C221.321 (7)C20—H200.9300
O5—C231.482 (8)C21—H210.9300
O6—C221.193 (7)C23—C241.471 (12)
O7—C301.308 (8)C23—H23A0.9700
O7—C311.453 (7)C23—H23B0.9700
O8—C301.209 (8)C24—H24A0.9600
C1—C21.391 (7)C24—H24B0.9600
C1—H10.9300C24—H24C0.9600
C2—C31.373 (7)C25—C261.374 (7)
C2—H20.9300C25—H250.9300
C3—C41.375 (7)C26—C271.395 (8)
C3—C61.467 (7)C26—H260.9300
C4—C51.375 (7)C27—C281.353 (7)
C4—H40.9300C27—C301.482 (8)
C5—H50.9300C28—C291.392 (8)
C7—C81.464 (9)C28—H280.9300
C7—H7A0.9700C29—H290.9300
C7—H7B0.9700C31—C321.488 (10)
C8—H8A0.9600C31—H31A0.9700
C8—H8B0.9600C31—H31B0.9700
C8—H8C0.9600C32—H32A0.9600
C9—C101.369 (8)C32—H32B0.9600
C9—H90.9300C32—H32C0.9600
C10—C111.356 (9)
N6—Co1—N5177.8 (2)O3—C14—C11112.5 (8)
N6—Co1—N390.12 (17)O3—C15—C16105 (3)
N5—Co1—N387.69 (17)O3—C15—H15A110.8
N6—Co1—N290.37 (18)C16—C15—H15A110.8
N5—Co1—N290.09 (18)O3—C15—H15B110.8
N3—Co1—N291.72 (16)C16—C15—H15B110.8
N6—Co1—N191.34 (17)H15A—C15—H15B108.9
N5—Co1—N190.87 (18)O3—C15'—C16'109 (8)
N3—Co1—N1175.75 (16)O3—C15'—H15C109.8
N2—Co1—N184.29 (16)C16'—C15'—H15C109.8
N6—Co1—N489.01 (17)O3—C15'—H15D109.8
N5—Co1—N490.62 (18)C16'—C15'—H15D109.8
N3—Co1—N490.65 (16)H15C—C15'—H15D108.2
N2—Co1—N4177.55 (18)C15'—C16'—H16D109.5
N1—Co1—N493.36 (16)C15'—C16'—H16E109.5
C1—N1—C5116.8 (5)H16D—C16'—H16E109.5
C1—N1—Co1122.3 (4)C15'—C16'—H16F109.5
C5—N1—Co1118.6 (4)H16D—C16'—H16F109.5
C13—N2—C9117.7 (5)H16E—C16'—H16F109.5
C13—N2—Co1123.0 (4)N3—C17—C18122.4 (5)
C9—N2—Co1119.0 (4)N3—C17—H17118.8
C17—N3—C21117.4 (5)C18—C17—H17118.8
C17—N3—Co1120.3 (3)C19—C18—C17118.8 (5)
C21—N3—Co1122.1 (4)C19—C18—H18120.6
C29—N4—C25116.6 (5)C17—C18—H18120.6
C29—N4—Co1120.8 (4)C20—C19—C18118.6 (5)
C25—N4—Co1122.5 (4)C20—C19—C22119.3 (5)
C33—N5—Co1162.0 (5)C18—C19—C22122.1 (6)
C34—N6—Co1160.2 (5)C21—C20—C19119.5 (5)
C6—O1—C7116.8 (5)C21—C20—H20120.3
C14—O3—C15'121 (2)C19—C20—H20120.3
C14—O3—C15110.5 (13)N3—C21—C20123.2 (5)
C15'—O3—C1542 (2)N3—C21—H21118.4
C22—O5—C23117.6 (5)C20—C21—H21118.4
C30—O7—C31118.0 (6)O6—C22—O5124.5 (6)
N1—C1—C2123.8 (5)O6—C22—C19123.0 (6)
N1—C1—H1118.1O5—C22—C19112.5 (6)
C2—C1—H1118.1C24—C23—O5111.1 (7)
C3—C2—C1118.3 (5)C24—C23—H23A109.4
C3—C2—H2120.8O5—C23—H23A109.4
C1—C2—H2120.8C24—C23—H23B109.4
C2—C3—C4118.4 (5)O5—C23—H23B109.4
C2—C3—C6123.0 (5)H23A—C23—H23B108.0
C4—C3—C6118.6 (5)C23—C24—H24A109.5
C3—C4—C5119.0 (5)C23—C24—H24B109.5
C3—C4—H4120.5H24A—C24—H24B109.5
C5—C4—H4120.5C23—C24—H24C109.5
N1—C5—C4123.6 (5)H24A—C24—H24C109.5
N1—C5—H5118.2H24B—C24—H24C109.5
C4—C5—H5118.2N4—C25—C26123.7 (6)
O2—C6—O1123.3 (5)N4—C25—H25118.2
O2—C6—C3123.1 (6)C26—C25—H25118.2
O1—C6—C3113.6 (5)C25—C26—C27119.1 (5)
O1—C7—C8112.0 (6)C25—C26—H26120.5
O1—C7—H7A109.2C27—C26—H26120.5
C8—C7—H7A109.2C28—C27—C26117.2 (5)
O1—C7—H7B109.2C28—C27—C30122.3 (6)
C8—C7—H7B109.2C26—C27—C30120.5 (6)
H7A—C7—H7B107.9C27—C28—C29119.8 (6)
C7—C8—H8A109.5C27—C28—H28120.1
C7—C8—H8B109.5C29—C28—H28120.1
H8A—C8—H8B109.5N4—C29—C28123.6 (6)
C7—C8—H8C109.5N4—C29—H29118.2
H8A—C8—H8C109.5C28—C29—H29118.2
H8B—C8—H8C109.5O8—C30—O7125.1 (6)
N2—C9—C10122.5 (6)O8—C30—C27121.9 (7)
N2—C9—H9118.8O7—C30—C27113.0 (6)
C10—C9—H9118.8O7—C31—C32106.3 (6)
C11—C10—C9119.6 (6)O7—C31—H31A110.5
C11—C10—H10120.2C32—C31—H31A110.5
C9—C10—H10120.2O7—C31—H31B110.5
C10—C11—C12119.5 (6)C32—C31—H31B110.5
C10—C11—C14117.0 (7)H31A—C31—H31B108.7
C12—C11—C14123.5 (7)C31—C32—H32A109.5
C11—C12—C13117.7 (6)C31—C32—H32B109.5
C11—C12—H12121.1H32A—C32—H32B109.5
C13—C12—H12121.1C31—C32—H32C109.5
N2—C13—C12123.0 (6)H32A—C32—H32C109.5
N2—C13—H13118.5H32B—C32—H32C109.5
C12—C13—H13118.5N5—C33—S1179.1 (6)
O4—C14—O3125.6 (9)N6—C34—S2176.5 (6)
O4—C14—C11121.8 (9)
N6—Co1—N1—C1161.4 (4)C4—C3—C6—O28.7 (9)
N5—Co1—N1—C118.4 (4)C2—C3—C6—O18.2 (8)
N3—Co1—N1—C189 (3)C4—C3—C6—O1174.0 (5)
N2—Co1—N1—C1108.4 (4)C6—O1—C7—C882.6 (7)
N4—Co1—N1—C172.3 (4)C13—N2—C9—C102.5 (9)
N6—Co1—N1—C536.5 (4)Co1—N2—C9—C10176.9 (5)
N5—Co1—N1—C5143.8 (4)N2—C9—C10—C112.0 (10)
N3—Co1—N1—C574 (3)C9—C10—C11—C120.3 (11)
N2—Co1—N1—C553.7 (4)C9—C10—C11—C14177.0 (7)
N4—Co1—N1—C5125.6 (4)C10—C11—C12—C130.7 (10)
N6—Co1—N2—C1325.3 (5)C14—C11—C12—C13175.8 (6)
N5—Co1—N2—C13152.5 (5)C9—N2—C13—C121.4 (9)
N3—Co1—N2—C1364.8 (5)Co1—N2—C13—C12175.6 (4)
N1—Co1—N2—C13116.7 (5)C11—C12—C13—N20.1 (9)
N4—Co1—N2—C13101 (5)C15'—O3—C14—O432 (4)
N6—Co1—N2—C9148.8 (4)C15—O3—C14—O414 (2)
N5—Co1—N2—C933.4 (5)C15'—O3—C14—C11144 (4)
N3—Co1—N2—C9121.1 (4)C15—O3—C14—C11169.8 (15)
N1—Co1—N2—C957.5 (4)C10—C11—C14—O42.2 (13)
N4—Co1—N2—C973 (5)C12—C11—C14—O4174.3 (9)
N6—Co1—N3—C1747.3 (4)C10—C11—C14—O3173.7 (8)
N5—Co1—N3—C17132.3 (4)C12—C11—C14—O39.7 (12)
N2—Co1—N3—C17137.7 (4)C14—O3—C15—C16137.8 (17)
N1—Co1—N3—C17157 (2)C15'—O3—C15—C1624 (3)
N4—Co1—N3—C1741.7 (4)C14—O3—C15'—C16'96 (4)
N6—Co1—N3—C21138.5 (4)C15—O3—C15'—C16'9 (3)
N5—Co1—N3—C2141.9 (4)C21—N3—C17—C183.6 (9)
N2—Co1—N3—C2148.1 (4)Co1—N3—C17—C18170.9 (5)
N1—Co1—N3—C2128 (3)N3—C17—C18—C191.9 (9)
N4—Co1—N3—C21132.5 (4)C17—C18—C19—C201.4 (9)
N6—Co1—N4—C29154.9 (4)C17—C18—C19—C22177.4 (6)
N5—Co1—N4—C2922.9 (4)C18—C19—C20—C212.9 (9)
N3—Co1—N4—C2964.8 (4)C22—C19—C20—C21175.9 (6)
N2—Co1—N4—C29130 (4)C17—N3—C21—C202.0 (9)
N1—Co1—N4—C29113.8 (4)Co1—N3—C21—C20172.4 (5)
N6—Co1—N4—C2521.5 (4)C19—C20—C21—N31.2 (9)
N5—Co1—N4—C25160.7 (4)C23—O5—C22—O61.3 (11)
N3—Co1—N4—C25111.6 (4)C23—O5—C22—C19178.2 (6)
N2—Co1—N4—C2554 (5)C20—C19—C22—O67.1 (10)
N1—Co1—N4—C2569.8 (4)C18—C19—C22—O6174.2 (7)
N6—Co1—N5—C3315 (6)C20—C19—C22—O5172.5 (6)
N3—Co1—N5—C334.7 (15)C18—C19—C22—O56.2 (9)
N2—Co1—N5—C3387.1 (15)C22—O5—C23—C2487.8 (9)
N1—Co1—N5—C33171.3 (15)C29—N4—C25—C260.2 (8)
N4—Co1—N5—C3395.3 (15)Co1—N4—C25—C26176.4 (4)
N5—Co1—N6—C34155 (5)N4—C25—C26—C271.1 (9)
N3—Co1—N6—C34165.0 (14)C25—C26—C27—C282.3 (8)
N2—Co1—N6—C34103.3 (14)C25—C26—C27—C30177.7 (5)
N1—Co1—N6—C3419.0 (14)C26—C27—C28—C292.4 (8)
N4—Co1—N6—C3474.3 (14)C30—C27—C28—C29177.7 (5)
C5—N1—C1—C22.0 (8)C25—N4—C29—C280.2 (8)
Co1—N1—C1—C2160.5 (4)Co1—N4—C29—C28176.4 (4)
N1—C1—C2—C30.5 (8)C27—C28—C29—N41.1 (9)
C1—C2—C3—C43.3 (8)C31—O7—C30—O81.2 (10)
C1—C2—C3—C6174.5 (5)C31—O7—C30—C27178.2 (5)
C2—C3—C4—C53.7 (8)C28—C27—C30—O8170.3 (6)
C6—C3—C4—C5174.3 (5)C26—C27—C30—O89.7 (9)
C1—N1—C5—C41.6 (8)C28—C27—C30—O79.1 (8)
Co1—N1—C5—C4161.5 (4)C26—C27—C30—O7170.9 (5)
C3—C4—C5—N11.2 (9)C30—O7—C31—C32175.2 (6)
C7—O1—C6—O22.4 (9)Co1—N5—C33—S1101 (39)
C7—O1—C6—C3179.7 (5)Co1—N6—C34—S227 (11)
C2—C3—C6—O2169.1 (6)

Experimental details

Crystal data
Chemical formula[Co(NCS)2(C8H9NO2)4]
Mr779.74
Crystal system, space groupMonoclinic, P21
Temperature (K)298
a, b, c (Å)11.2190 (11), 14.3742 (16), 12.0189 (13)
β (°) 96.430 (1)
V3)1926.0 (4)
Z2
Radiation typeMo Kα
µ (mm1)0.61
Crystal size (mm)0.48 × 0.40 × 0.30
Data collection
DiffractometerBruker SMART 1000 CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2002)
Tmin, Tmax0.759, 0.838
No. of measured, independent and
observed [I > 2σ(I)] reflections
10061, 5985, 4025
Rint0.037
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.122, 1.03
No. of reflections5985
No. of parameters484
No. of restraints1
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.37, 0.28
Absolute structureFlack (1983), 2433 Friedel pairs
Absolute structure parameter0.04 (2)

Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

The authors appreciate the help of Professor Dr Hongyou Guo and the financial support of the Science Foundation of Huaihua University (grant No. HHUQ.2009–10.).

References

First citationBruker (2002). SAINT, SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationDiehr, S., Wöhlert, S., Boeckmann, J. & Näther, C. (2011). Acta Cryst. E67, m1898.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationManna, S. C., Jana, A. D., Drew, M. G. B. & Mostafa, G. (2008). Polyhedron, 27, 1280–1286.  Web of Science CSD CrossRef CAS Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWang, N., Sun, X., Wan, D., Chen, J. & Li, B. (2012). Acta Cryst. E68, m204–m205.  Web of Science CSD CrossRef IUCr Journals Google Scholar

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