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Volume 68 
Part 1 
Page m20  
January 2012  

Received 7 November 2011
Accepted 29 November 2011
Online 7 December 2011

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.003 Å
R = 0.028
wR = 0.076
Data-to-parameter ratio = 13.0
Details
Open access

Chloridobis(dimethylglyoximato-[kappa]2N,N')(ethyl pyridine-3-carboxylate-[kappa]N)cobalt(III)

aHenan University of Technology, School of Chemistry and Chemical Engineering, Zhengzhou 450001, People's Republic of China
Correspondence e-mail: ssdyok@yahoo.com.cn

In the title compound, [Co(C4H7N2O2)2Cl(C8H9NO2)], which was prepared as a model complex of vitamin B12, the CoIII atom, which is linked to four N atoms of the pseudo-macrocyclic (dmgH)2 ligand (dmgH is dimethylglyoximate) in the equatorial plane and one Cl- anion and one N atom of ethyl nicotinate in apical positions, displays an approximately octahedral coordination. The Co atom is 0.0187 (8) Å out of the mean plane of the four equatorial N atoms. The structure has an O...H...O bridge, which is very common in cobaloxime derivatives, with O...H distances of 1.24 (2) and 1.25 (2) Å.

Related literature

For background to the chemistry of cobaloximes, see: Schrayzer (1968[Schrayzer, G. N. (1968). Acc. Chem. Res. 1, 97-103.]); Zangrando et al. (2003[Zangrando, E., Trani, M., Stabon, E., Carfagna, C., Milani, B. & Mestroni, G. (2003). Eur. J. Inorg. Chem. pp. 2683-2692.]). For applications of cobaloximes in proton reduction, see: Razavet et al. (2005[Razavet, M., Artero, V. & Fontecave, M. (2005). Inorg. Chem. 44, 4786-4795.]). For related structures, see: Mandal & Gupta (2005[Mandal, D. & Gupta, B. D. (2005). Organometallics, 24, 1501-1510.], 2007[Mandal, D. & Gupta, B. D. (2007). Organometallics, 26, 658-670.]); Bhuyan et al. (2007[Bhuyan, M., Laskar, M., Mandal, D. & Gupta, B. D. (2007). Organometallics, 26, 3559-3567.]); Dutta et al. (2009[Dutta, G., Kumar, K. & Gupta, B. D. (2009). Organometallics, 28, 3485-3491.]). For NMR research on O...H...O bridges, see: Bakac & Espenson (1984[Bakac, A. & Espenson, J. H. (1984). J. Am. Chem. Soc. 106, 5197-5202.]). For deprotonation of O...H...O bridges by BF3·Et2O, see: Magnuson & Weber (1974[Magnuson, V. E. & Weber, J. H. (1974). J. Organomet. Chem. 74, 135-141.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(C4H7N2O2)2Cl(C8H9NO2)]

  • Mr = 475.77

  • Monoclinic, P 21 /c

  • a = 8.1961 (11) Å

  • b = 14.2224 (19) Å

  • c = 17.365 (2) Å

  • [beta] = 98.340 (2)°

  • V = 2002.8 (5) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.03 mm-1

  • T = 293 K

  • 0.32 × 0.15 × 0.06 mm

Data collection
  • Bruker APEXII area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.830, Tmax = 0.940

  • 9364 measured reflections

  • 3532 independent reflections

  • 3104 reflections with I > 2[sigma](I)

  • Rint = 0.020

Refinement
  • R[F2 > 2[sigma](F2)] = 0.028

  • wR(F2) = 0.076

  • S = 1.10

  • 3532 reflections

  • 272 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.27 e Å-3

  • [Delta][rho]min = -0.28 e Å-3

Table 1
Selected bond lengths (Å)

Co1-Cl1 2.2326 (6)
Co1-N1 1.8925 (16)
Co1-N2 1.8872 (16)
Co1-N3 1.8970 (16)
Co1-N4 1.9020 (16)
Co1-N5 1.9701 (15)

Data collection: APEX2 (Bruker, 2007[Bruker (2007). SAINT-Plus and APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2007[Bruker (2007). SAINT-Plus and APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; 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: SHELXL97.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: VN2023 ).


Acknowledgements

We are grateful to the Chinese National Natural Science Foundation (grant No. 21101057) and the Doctoral Fund of Henan University of Technology (No. 150389).

References

Bakac, A. & Espenson, J. H. (1984). J. Am. Chem. Soc. 106, 5197-5202.  [CrossRef] [ChemPort] [ISI]
Bhuyan, M., Laskar, M., Mandal, D. & Gupta, B. D. (2007). Organometallics, 26, 3559-3567.  [CSD] [CrossRef] [ChemPort]
Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2007). SAINT-Plus and APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Dutta, G., Kumar, K. & Gupta, B. D. (2009). Organometallics, 28, 3485-3491.  [CSD] [CrossRef] [ChemPort]
Magnuson, V. E. & Weber, J. H. (1974). J. Organomet. Chem. 74, 135-141.  [CrossRef] [ChemPort]
Mandal, D. & Gupta, B. D. (2005). Organometallics, 24, 1501-1510.  [CSD] [CrossRef] [ChemPort]
Mandal, D. & Gupta, B. D. (2007). Organometallics, 26, 658-670.  [CSD] [CrossRef] [ChemPort]
Razavet, M., Artero, V. & Fontecave, M. (2005). Inorg. Chem. 44, 4786-4795.  [ISI] [CrossRef] [PubMed] [ChemPort]
Schrayzer, G. N. (1968). Acc. Chem. Res. 1, 97-103.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Zangrando, E., Trani, M., Stabon, E., Carfagna, C., Milani, B. & Mestroni, G. (2003). Eur. J. Inorg. Chem. pp. 2683-2692.  [ISI] [CSD] [CrossRef]


Acta Cryst (2012). E68, m20  [ doi:10.1107/S1600536811051397 ]

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