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Volume 64 
Part 10 
Pages m1264-m1265  
October 2008  

Received 20 August 2008
Accepted 8 September 2008
Online 13 September 2008

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Key indicators
Single-crystal X-ray study
T = 273 K
Mean [sigma](C-C) = 0.006 Å
R = 0.041
wR = 0.109
Data-to-parameter ratio = 15.4
Details
Open access

Bis(diethylenetriamine-[kappa]3N,N',N'')nickel(II) bis(1,2-dicyanoethene-1,2-dithiolato-[kappa]2S,S')nickel(II)

Dao-Peng Zhang,a Hai-Long Wang,a Li-Fang Zhanga* and Zhong-Hai Nia

aSchool of Chemistry & Chemical Technology, Shandong University, Jinan 250100, People's Republic of China
Correspondence e-mail: Zhanglf@sdu.edu.cn

The title compound, [Ni(C4H13N3)2][Ni(C4N2S2)2], has been synthesized by the reaction of Ni(ClO4)2·6H2O, diethylenetriamine (deta) and Na2[Ni(mnt)2] [mnt = maleonitriledithiolate(2-)] in methanol. The structure is composed of a [Ni(deta)2]2+ cation and a [Ni(mnt)2]2- anion. The coordination geometry of the NiII ion in the cation is slightly distorted octahedral, defined by six N atoms from two deta ligands, while the NiII ion in the anion is four-coordinated by four S atoms from two mnt ligands in a slightly distorted square-planar geometry. The cations and anions are connected by N-H...N hydrogen bonds.

Related literature

For related literature, see: Bois et al. (1998[Bois, H., Connelly, N. G., Crossley, J. G., Guillorit, J., Lewis, G. R., Orpen, A. G. & Thornton, P. (1998). J. Chem. Soc. Dalton Trans. pp. 2833-2838.]); Keum et al. (1992[Keum, C., Kim, C., Kim, C., Kwak, H., Kwon, M. & Namgung, H. (1992). Bull. Korean. Chem. Soc. 13, 695-699.]); Miller et al. (1989[Miller, J. S., Calabrese, J. C. & Epstein, A. J. (1989). Inorg. Chem. 28, 4230-4238.]); Ren et al. (2001[Ren, X.-M., Duan, C.-Y., Zhu, H.-Z., Meng, Q.-J., Hu, C.-J., Lu, C.-S. & Liu, Y.-J. (2001). Transition Met. Chem. 26, 295-299.]); Robertson & Cronin (2002[Robertson, N. & Cronin, L. (2002). Coord. Chem. Rev. 227, 93-127.]); Simmons et al. (1962[Simmons, H. E., Vest, R. D., Blomstrom, D. C., Roland, J. R. & Cairns, T. L. (1962). J. Am. Chem. Soc. 84, 4746-4756.]).

[Scheme 1]

Experimental

Crystal data

  • [Ni(C4H13N3)2][Ni(C4N2S2)2]

  • Mr = 604.13

  • Monoclinic, P 21 /n

  • a = 9.589 (3) Å

  • b = 16.910 (5) Å

  • c = 16.146 (4) Å

  • [beta] = 97.491 (4)°

  • V = 2595.8 (13) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.80 mm-1

  • T = 273 (2) K

  • 0.19 × 0.17 × 0.15 mm
Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.717, Tmax = 0.766

  • 13610 measured reflections

  • 5065 independent reflections

  • 3393 reflections with I > 2[sigma](I)

  • Rint = 0.037
Refinement

  • R[F2 > 2[sigma](F2)] = 0.041

  • wR(F2) = 0.109

  • S = 0.99

  • 5065 reflections

  • 329 parameters

  • 10 restraints

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

  • [Delta][rho]max = 0.86 e Å-3

  • [Delta][rho]min = -0.26 e Å-3

Table 1
Selected geometric parameters (Å, °)

Ni1-S1 2.1739 (12)
Ni1-S2 2.1617 (12)
Ni1-S3 2.1732 (12)
Ni1-S4 2.1658 (12)
Ni2-N5 2.164 (3)
Ni2-N6 2.065 (3)
Ni2-N7 2.150 (4)
Ni2-N8 2.145 (3)
Ni2-N9 2.071 (4)
Ni2-N10 2.151 (3)
S2-Ni1-S4 87.98 (5)
S2-Ni1-S3 168.77 (5)
S4-Ni1-S3 92.72 (4)
S2-Ni1-S1 92.58 (4)
S4-Ni1-S1 170.10 (4)
S3-Ni1-S1 88.65 (4)
N6-Ni2-N9 177.56 (15)
N6-Ni2-N8 98.00 (14)
N9-Ni2-N8 81.73 (14)
N6-Ni2-N7 82.24 (16)
N9-Ni2-N7 95.37 (17)
N8-Ni2-N7 95.96 (15)
N6-Ni2-N10 98.69 (14)
N9-Ni2-N10 81.72 (14)
N8-Ni2-N10 163.04 (16)
N7-Ni2-N10 89.25 (16)
N6-Ni2-N5 81.47 (14)
N9-Ni2-N5 100.96 (15)
N8-Ni2-N5 91.32 (13)
N7-Ni2-N5 162.93 (16)
N10-Ni2-N5 88.20 (14)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N5-H5A...N4i 0.86 (3) 2.30 (4) 3.098 (6) 154 (3)
N5-H5B...N2ii 0.86 (3) 2.48 (3) 3.186 (5) 140 (4)
N7-H7A...N3iii 0.86 (4) 2.56 (3) 3.207 (7) 134 (3)
N8-H8B...N3iii 0.86 (3) 2.48 (4) 3.164 (6) 138 (3)
N9-H9A...N1iv 0.86 (2) 2.58 (3) 3.387 (6) 156 (5)
N10-H10C...N2ii 0.87 (3) 2.34 (3) 3.198 (5) 173 (5)
Symmetry codes: (i) -x+1, -y+1, -z; (ii) [x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]; (iii) x+1, y, z; (iv) [-x+{\script{5\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}].

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

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2151 ).

Acknowledgements

This work was supported by the Natural Science Foundation of China (No. 20701027) and the Postdoctoral Scientific Foundation of China (No. 200704211076).

References

Bois, H., Connelly, N. G., Crossley, J. G., Guillorit, J., Lewis, G. R., Orpen, A. G. & Thornton, P. (1998). J. Chem. Soc. Dalton Trans. pp. 2833-2838.  [CrossRef]
Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.
Keum, C., Kim, C., Kim, C., Kwak, H., Kwon, M. & Namgung, H. (1992). Bull. Korean. Chem. Soc. 13, 695-699.  [ChemPort]
Miller, J. S., Calabrese, J. C. & Epstein, A. J. (1989). Inorg. Chem. 28, 4230-4238.  [CrossRef] [ChemPort]
Ren, X.-M., Duan, C.-Y., Zhu, H.-Z., Meng, Q.-J., Hu, C.-J., Lu, C.-S. & Liu, Y.-J. (2001). Transition Met. Chem. 26, 295-299.  [CrossRef] [ChemPort]
Robertson, N. & Cronin, L. (2002). Coord. Chem. Rev. 227, 93-127.  [ISI] [CrossRef] [ChemPort]
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Simmons, H. E., Vest, R. D., Blomstrom, D. C., Roland, J. R. & Cairns, T. L. (1962). J. Am. Chem. Soc. 84, 4746-4756.  [CrossRef] [ChemPort]

Acta Cryst (2008). E64, m1264-m1265   [ doi:10.1107/S1600536808028663 ]

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