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Volume 69 
Part 1 
Page m59  
January 2013  

Received 14 November 2012
Accepted 12 December 2012
Online 15 December 2012

Key indicators
Single-crystal X-ray study
T = 200 K
Mean [sigma](C-C) = 0.004 Å
R = 0.037
wR = 0.084
Data-to-parameter ratio = 20.9
Details
Open access

Bis(4,4'-sulfanediyldipyridinium) tetrachloridonickelate(II) dichloride

aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany
Correspondence e-mail: jwerner@ac.uni-kiel.de

In the title compound, (C10H10N2S)2[NiCl4]Cl2, the Ni2+ cation is tetrahedrally coordinated by four chloride anions. Two 4,4'-sulfanediyldipyridinium cations and two non-coordinating chloride anions are connected via N-H...Cl hydrogen-bonding interactions into 20-membered rings, in the middle of which are situated the [NiCl4]2- complex anions. These rings are stacked in the b-axis direction. The Ni2+ cation is located on a twofold rotation axis, whereas the chloride anions and the 4,4'-sulfanediyldipyridinium cations occupy general positions.

Related literature

For background information on this project, see: Boeckmann & Näther (2010[Boeckmann, J. & Näther, C. (2010). Dalton Trans. 39, 11019-11026.], 2011[Boeckmann, J. & Näther, C. (2011). Chem. Commun. 47, 7104-7106.]); Wöhlert et al. (2011[Wöhlert, S., Boeckmann, J., Wriedt, M. & Näther, C. (2011). Angew. Chem. Int. Ed. 50, 6920-6923.]). For the crystal structure of 4,4'-thiodipyridine, see: Vaganova et al. (2004[Vaganova, E., Wachtel, E., Rozenberg, H., Khodorkovsky, V., Leitus, V., Shimon, L., Reich, S. & Yitzchaik, S. (2004). Chem. Mater. 16, 3976-3979.]).

[Scheme 1]

Experimental

Crystal data
  • (C10H10N2S)2[NiCl4]Cl2

  • Mr = 651.93

  • Monoclinic, C 2/c

  • a = 19.0497 (9) Å

  • b = 8.0534 (5) Å

  • c = 17.7883 (11) Å

  • [beta] = 92.368 (6)°

  • V = 2726.7 (3) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.47 mm-1

  • T = 200 K

  • 0.32 × 0.13 × 0.07 mm

Data collection
  • Stoe IPDS-1 diffractometer

  • Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]) Tmin = 0.789, Tmax = 0.899

  • 10707 measured reflections

  • 3162 independent reflections

  • 2308 reflections with I > 2[sigma](I)

  • Rint = 0.062

Refinement
  • R[F2 > 2[sigma](F2)] = 0.037

  • wR(F2) = 0.084

  • S = 0.99

  • 3162 reflections

  • 151 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.47 e Å-3

  • [Delta][rho]min = -0.43 e Å-3

Table 1
Selected bond lengths (Å)

Ni1-Cl1 2.2569 (7)
Ni1-Cl2 2.2706 (6)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N2-H1N2...Cl3i 0.88 2.12 2.987 (3) 168
N1-H1N1...Cl3 0.88 2.32 3.078 (3) 144
Symmetry code: (i) [-x+1, y, -z+{\script{3\over 2}}].

Data collection: X-AREA (Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; 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: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and DIAMOND (Brandenburg, 2011[Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2703 ).


Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. NA 720/3-1) and the State of Schleswig-Holstein. We thank Professor Dr Wolfgang Bensch for access to his experimental facilities.

References

Boeckmann, J. & Näther, C. (2010). Dalton Trans. 39, 11019-11026.  [CSD] [CrossRef] [ChemPort] [PubMed]
Boeckmann, J. & Näther, C. (2011). Chem. Commun. 47, 7104-7106.  [CSD] [CrossRef] [ChemPort]
Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.
Vaganova, E., Wachtel, E., Rozenberg, H., Khodorkovsky, V., Leitus, V., Shimon, L., Reich, S. & Yitzchaik, S. (2004). Chem. Mater. 16, 3976-3979.  [ISI] [CSD] [CrossRef] [ChemPort]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]
Wöhlert, S., Boeckmann, J., Wriedt, M. & Näther, C. (2011). Angew. Chem. Int. Ed. 50, 6920-6923.


Acta Cryst (2013). E69, m59  [ doi:10.1107/S1600536812050623 ]

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