Bis(3,5,7-triaza-1-azoniatricyclo­[3.3.1.13,7]deca­ne) bis­(1,2-dicyano­ethene-1,2-dithiol­ato)nickelate(II)

Pan, C.; Cai, B.; Pei, W.-B.

doi:10.1107/S160053681101645X

Volume 67
Part 6
Page m730
June 2011

Received 13 April 2011
Accepted 30 April 2011
Online 7 May 2011

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.004 Å
R = 0.038
wR = 0.075
Data-to-parameter ratio = 14.6
Details

Bis(3,5,7-triaza-1-azoniatricyclo[3.3.1.1^3,7]decane) bis(1,2-dicyanoethene-1,2-dithiolato)nickelate(II)

Chen Pan,^a Bin Cai ^a and Wen-Bo Pei ^a ^*

^aDepartment of Applied Chemistry, College of Science, Nanjing University of Technology, Nanjing 210009, People's Republic of China
Correspondence e-mail: peiwenbo@163.com

The asymmetric unit of the title complex, (C₆H₁₃N₄)₂[Ni(C₄N₂S₂)₂], comprises one 1-azonia-3,5,7-triazatricyclo[3.3.1.1^3,7]decane cation and one half of an [Ni(mnt)₂]^2- (mnt^2- is maleonitriledithiolate or 1,2-dicyanoethene-1,2-dithiolate) dianion. The Ni²⁺ ion is located on a center of inversion and is coordinated by four S atoms from two mnt^2- ligands in a square-planar coordination mode. Intermolecular N-HN hydrogen-bond interactions link one anion and two cations in the crystal structure.

Related literature

For general background to square-planar M[dithiolene]₂ complexes acting as magnetic materials or showing non-linear optical properties, see: Duan et al. (2010). For the synthesis, see: Pei et al. (2010). For related structures, see: Ren et al. (2002). For related literature on spectroscopic properties, see: Bigoli et al. (2002).

Experimental

Crystal data

(C₆H₁₃N₄)₂[Ni(C₄N₂S₂)₂]
M_r = 621.50
Monoclinic, P 2₁ /n
a = 10.2274 (9) Å
b = 10.7676 (10) Å
c = 12.7030 (11) Å
= 112.212 (2)°
V = 1295.1 (2) Å³
Z = 2
Mo K radiation
= 1.11 mm^-1
T = 296 K
0.20 × 0.15 × 0.15 mm

Data collection

Siemens SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick 2002) T_min = 0.819, T_max = 0.847
7528 measured reflections
2530 independent reflections
1784 reflections with I > 2(I)
R_int = 0.049

Refinement

R[F² > 2(F²)] = 0.038
wR(F²) = 0.075
S = 1.00
2530 reflections
173 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 0.48 e Å^-3
_min = -0.33 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N6-H1N1ⁱ	0.87 (4)	2.37 (4)	2.941 (5)	124 (3)
Symmetry code: (i) $[-x+{\script{1\over 2}}, y-{\script{3\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; 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.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IM2281 ).

Acknowledgements

The authors thank the Doctorial Innovation Fund of Nanjing University of Technology (grant No. BSCX200908).

References

Bigoli, F., Deplano, P., Mercuri, M. L., Pellinghelli, M. A., Pilia, L., Pintus, G., Serpe, A. & Trogu, E. F. (2002). Inorg. Chem. 41, 5241-5248.
Duan, H. B., Ren, X. M. & Meng, Q. J. (2010). Coord. Chem. Rev. 254, 1509-1522.
Pei, W. B., Wu, J. S., Liu, J. L., Ren, X. M. & Shen, L. J. (2010). Spectrochim. Acta Part A, 75, 191-197.
Ren, X. M., Meng, Q. J., Song, Y., Hu, C. J., Lu, C. S., Chen, X. Y. & Xue, Z. L. (2002). Inorg. Chem. 41, 5931-5933.
Sheldrick, G. M. (2002). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Siemens (1996). SMART and SAINT. Siemens Analytical X-ray Instrument Inc., Madison, Wisconsin, USA.

metal-organic compounds

Bis(3,5,7-triaza-1-azoniatricyclo[3.3.1.13,7]decane) bis(1,2-dicyanoethene-1,2-dithiolato)nickelate(II)