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

Werner, J.; Jess, I.; Näther, C.

doi:10.1107/S1600536812050623

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 (C-C) = 0.004 Å
R = 0.037
wR = 0.084
Data-to-parameter ratio = 20.9
Details

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

Julia Werner,^a ^* Inke Jess ^a and Christian Näther ^a

^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-HCl 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, 2011); Wöhlert et al. (2011). For the crystal structure of 4,4'-thiodipyridine, see: Vaganova et al. (2004).

Experimental

Crystal data

(C₁₀H₁₀N₂S)₂[NiCl₄]Cl₂
M_r = 651.93
Monoclinic, C 2/c
a = 19.0497 (9) Å
b = 8.0534 (5) Å
c = 17.7883 (11) Å
= 92.368 (6)°
V = 2726.7 (3) Å³
Z = 4
Mo K radiation
= 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) T_min = 0.789, T_max = 0.899
10707 measured reflections
3162 independent reflections
2308 reflections with I > 2(I)
R_int = 0.062

Refinement

R[F² > 2(F²)] = 0.037
wR(F²) = 0.084
S = 0.99
3162 reflections
151 parameters
H-atom parameters constrained
_max = 0.47 e Å^-3
_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-HA	D-H	HA	DA	D-HA
N2-H1N2Cl3ⁱ	0.88	2.12	2.987 (3)	168
N1-H1N1Cl3	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); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011); software used to prepare material for publication: publCIF (Westrip, 2010).

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.
Boeckmann, J. & Näther, C. (2011). Chem. Commun. 47, 7104-7106.
Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
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.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
Wöhlert, S., Boeckmann, J., Wriedt, M. & Näther, C. (2011). Angew. Chem. Int. Ed. 50, 6920-6923.

metal-organic compounds