Tris(1,2-diamino­ethane)­nickel(II) hexa­fluoridosilicate

Haníková, J.; Kuchár, J.; Černák, J.; Pelosi, G.

doi:10.1107/S1600536810041553

Volume 66
Part 11
Pages m1451-m1452
November 2010

Received 9 September 2010
Accepted 14 October 2010
Online 23 October 2010

Key indicators
Single-crystal X-ray study
T = 291 K
Mean (C-C) = 0.003 Å
R = 0.027
wR = 0.064
Data-to-parameter ratio = 16.8
Details

Tris(1,2-diaminoethane)nickel(II) hexafluoridosilicate

Jaroslava Haníková,^a ^* Juraj Kuchár,^a Juraj Cernák ^a and Giorgio Pelosi ^b

^aDepartment of Inorganic Chemistry, Institute of Chemistry, P. J. Safárik University, Moyzesova 11, 041 54 Kosice, Slovakia, and ^bDipartimento di Chimica Generale ed Inorganica, Universitá di Parma, Viale della Scienze, 43124 Parma, Italy
Correspondence e-mail: jaroslava.hanikova@student.upjs.sk

The ionic title complex, [Ni(C₂H₈N₂)₃](SiF₆), is built up of [Ni(en)₃]²⁺ complex cations (en = 1,2-diaminoethane) and hexafluoridosilicate anions. Single crystals of the title complex were isolated from an aqueous-ethanolic Ni²⁺-en-SiF₆^2- system. The Ni(II) and Si atoms are each located on a special position with site symmetry 3.2. The Ni(II) atom coordination sphere is octahedrally deformed, being coordinated by three chelating diamine ligands with an Ni-N distance of 2.1233 (18) Å. The crystal packing of the respective ions corresponds to the structure type of the hexagonal form of BN. Beside ionic forces, the packing is governed by N-HF hydrogen bonds, which lead to the formation of hydrophobic channels running along the 6₃ screw axis. The structure was refined as an inversion twin [0.49 (3): 0.51 (3)].

Related literature

For the hexafluoridosilicate anion acting as simple counter-ion, see: Li et al. (2009). For two nickel(II) complexes containing the hexafluoridosilicate anion as counter-ion, see: Spek et al. (1988); Wu et al. (2008). For complexes containing the [Ni(en)₃]²⁺ complex cation and hexafluorido-type anions, see: Pan et al. (2005); Ribas et al. (1998); James et al. (1998); Contakes et al. (2000).

Experimental

Crystal data

[Ni(C₂H₈N₂)₃](SiF₆)
M_r = 381.11
Hexagonal, P 6₃ 22
a = 9.1670 (9) Å
c = 9.763 (1) Å
V = 710.51 (12) Å³
Z = 2
Mo K radiation
= 1.52 mm^-1
T = 291 K
0.42 × 0.21 × 0.15 mm

Data collection

Oxford Diffraction Xcalibur diffractometer with Sapphire2 detector
Absorption correction: numerical [Clark & Reid (1995) in CrysAlis PRO (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Abingdon, England.]$ )] T_min = 0.834, T_max = 0.859
8628 measured reflections
554 independent reflections
489 reflections with I > 2(I)
R_int = 0.050

Refinement

R[F² > 2(F²)] = 0.027
wR(F²) = 0.064
S = 1.07
554 reflections
33 parameters
H-atom parameters constrained
_max = 0.68 e Å^-3
_min = -0.19 e Å^-3
Absolute structure: Flack (1983), 89 Friedel pairs
Flack parameter: 0.49 (3)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1F1ⁱ	0.90	2.30	3.137 (2)	154
N1-H1F1ⁱⁱ	0.90	2.48	3.235 (2)	142
N1-H2F1ⁱⁱⁱ	0.90	2.25	3.137 (2)	167
Symmetry codes: (i) y, x, -z; (ii) -x+1, -x+y+1, -z; (iii) -x+y+1, -x+1, z.

Data collection: CrysAlis PRO (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Abingdon, England.]$ ); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Crystal Impact, 2007); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2212 ).

Acknowledgements

This work was supported by the Slovak grant agencies VEGA (grant 1/0089/09) and APVV (contract Nos. APVV-VVCE-0058-07 and APVV-0006-07). Support from P. J. Safárik University (VVGS PF 19/2010/CH) is also gratefully acknowledged. We thank student M. Adam for help with the experimental work.

References

Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.
Contakes, S. M., Klausmeyer, K. K. & Rauchfuss, T. B. (2000). Inorg. Chem. 39, 2069-2075.
Crystal Impact (2007). DIAMOND. Crystal Impact, Bonn, Germany.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
James, M., Kawaguchi, H. & Tatsumi, K. (1998). Polyhedron, 17, 1571-1577.
Li, Y., Shi, Q., Slawin, A. M. Z., Woollins, J. D. & Dong, J. (2009). Acta Cryst. E65, m1522.
Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Abingdon, England.
Pan, Q.-H., Li, J.-Y., Yu, J.-H., Wang, Y., Fang, Q.-R. & Xu, R.-R. (2005). Gaodeng Xuexiao Huaxue Xuebao, 26, 2199-2200.
Ribas, J., Monfort, M., Resino, I., Ghosh, B. K., Solans, X. & Font-Bardia, M. (1998). Polyhedron, 17, 1735-1739.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L., Duisenberg, A. J. M., Bouwman, E., Driessen, W. L. & Reedijk, J. (1988). Acta Cryst. C44, 1569-1572.
Wu, L.-P., Zhao, S.-M., Zhang, G.-F. & Ng, S. W. (2008). Acta Cryst. E64, m802.

metal-organic compounds