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Volume 68 
Part 1 
Page m40  
January 2012  

Received 8 November 2011
Accepted 6 December 2011
Online 10 December 2011

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Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.004 Å
R = 0.041
wR = 0.100
Data-to-parameter ratio = 12.3
Details
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Bis[[mu]3-N'-oxidopyridine-2-carboximidamidato(2-)]bis[[mu]2-N'-oxidopyridine-2-carboximidamidato(1-)]tetrapyridinetetranickel(II) dinitrate

Xiao-Hui Denga* and Jing-Wen Ranb

aInstitute of Cash Crops, Hubei Academy of Agricultural Science, Wuhan 430064, People's Republic of China, and bKey Laboratory of Industrial Ecology and Environmental Engineering (MOE) and State Key Laboratory of Fine Chemicals, School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, People's Republic of China
Correspondence e-mail: xhdengyy@yahoo.com.cn

The title compound, [Ni4(C6H5N3O)2(C6H6N3O)2(C5H5N)4](NO3)2, is a tetranuclear nickel complex containing a single-decker cation, located on an inversion center. The two unique NiII cations are N,N',N'',O-chelated by carboximidamidate(2-) and carboximidamidate(1-) anions, forming a distorted four-coordinate planar structure, while the other two NiII atoms are N,N',O,O'-chelated by the same bridging ligands and two pyridine molecules, affording six-coordinated metals in an octahedral geometry. The cation is isostructural with the complex crystallized with perchlorate counter-ions in place of nitrate.

Related literature

For similar metal complexes, see: Kou et al. (2010[Kou, H.-Z., An, G.-Y., Ji, C.-M., Wang, B.-W. & Cui, A.-L. (2010). Dalton Trans. 39, 9604-9610.]); Papatriantafyllopoulou et al. (2008[Papatriantafyllopoulou, C., Jones, L. F., Nguyen, T. D., Matamoros-Salvador, N., Cunha-Silva, L., Almeida Paz, F. A., Rocha, J., Evangelisti, M., Brechin, E. K. & Perlepes, S. P. (2008). Dalton Trans. pp. 3153-3155.]); Inglis et al. (2010[Inglis, R., Stoumpos, C. C., Prescimone, A., Siczek, M., Lis, T., Wernsdorfer, W., Brechin, E. K. & Milios, C. J. (2010). Dalton Trans. 39, 4777-4785.]); Deng & Ran (2011[Deng, X.-H. & Ran, J.-W. (2011). Acta Cryst. E67, m1323-m1324.]). For the synthesis of the ligand pyridine-2-amidoxine, see: Bernasek (1957[Bernasek, E. (1957). J. Org. Chem. 22, 1263-1263.]).

[Scheme 1]

Experimental

Crystal data

  • [Ni4(C6H5N3O)2(C6H6N3O)2(C5H5N)4](NO3)2

  • Mr = 1217.80

  • Triclinic, [P \overline 1]

  • a = 10.4356 (6) Å

  • b = 10.7190 (8) Å

  • c = 11.2908 (9) Å

  • [alpha] = 92.041 (6)°

  • [beta] = 98.240 (5)°

  • [gamma] = 100.870 (5)°

  • V = 1224.96 (15) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 1.59 mm-1

  • T = 293 K

  • 0.40 × 0.38 × 0.35 mm
Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2007[Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.569, Tmax = 0.606

  • 9481 measured reflections

  • 4286 independent reflections

  • 3180 reflections with I > 2[sigma](I)

  • Rint = 0.039
Refinement

  • R[F2 > 2[sigma](F2)] = 0.041

  • wR(F2) = 0.100

  • S = 1.03

  • 4286 reflections

  • 349 parameters

  • 8 restraints

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

  • [Delta][rho]max = 0.66 e Å-3

  • [Delta][rho]min = -0.52 e Å-3

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2, SAINT 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.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BH2397 ).

Acknowledgements

This research was supported by the Natural Science Fund of Hubei Province (project ZRZ0140) and the National Natural Science Foundation of China (Nos. 20877013 and 20837001). The authors thank Professor Z.-M. Qiu of Hubei Academy of Agricultural Science for his valuable suggestions.

References

Bernasek, E. (1957). J. Org. Chem. 22, 1263-1263.  [CrossRef] [ChemPort]
Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Deng, X.-H. & Ran, J.-W. (2011). Acta Cryst. E67, m1323-m1324.  [CSD] [CrossRef] [details]
Inglis, R., Stoumpos, C. C., Prescimone, A., Siczek, M., Lis, T., Wernsdorfer, W., Brechin, E. K. & Milios, C. J. (2010). Dalton Trans. 39, 4777-4785.  [CSD] [CrossRef] [ChemPort] [PubMed]
Kou, H.-Z., An, G.-Y., Ji, C.-M., Wang, B.-W. & Cui, A.-L. (2010). Dalton Trans. 39, 9604-9610.  [CSD] [CrossRef] [ChemPort] [PubMed]
Papatriantafyllopoulou, C., Jones, L. F., Nguyen, T. D., Matamoros-Salvador, N., Cunha-Silva, L., Almeida Paz, F. A., Rocha, J., Evangelisti, M., Brechin, E. K. & Perlepes, S. P. (2008). Dalton Trans. pp. 3153-3155.  [CSD] [CrossRef]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]

Acta Cryst (2012). E68, m40  [ doi:10.1107/S1600536811052524 ]

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