trans-Bis(acetonitrile-κN)tetra­aqua­cobalt(II) tetra­chloridocobaltate(II)

Patroniak, V.; Kubicki, M.

doi:10.1107/S1600536809000750

Volume 65
Part 2
Pages m173-m174
February 2009

Received 10 December 2008
Accepted 7 January 2009
Online 10 January 2009

Key indicators
Single-crystal X-ray study
T = 170 K
Mean (C-C) = 0.011 Å
R = 0.064
wR = 0.164
Data-to-parameter ratio = 18.1
Details

trans-Bis(acetonitrile-N)tetraaquacobalt(II) tetrachloridocobaltate(II)

Violetta Patroniak ^a and Maciej Kubicki ^a ^*

^aDepartment of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan, Poland
Correspondence e-mail: mkubicki@amu.edu.pl

In the title complex, [Co(CH₃CN)₂(H₂O)₄][CoCl₄], the Co^II ions are octahedrally coordinated in the cation, with trans-disposed acetonitrile ligands, and tetrahedrally coordinated in the anion. An extensive network of O-H(water)Cl hydrogen bonds between cations and anions connects the ions into a three-dimensional network. The Co-Cl distances correlate with the number of hydrogen bonds accepted by the Cl atoms.

Related literature

For background to our studies on new helical metal complexes, see: Stefankiewicz et al. (2008). There are only few examples of other bis(acetonitrile)tetraaqua complexes, these are mainly cobalt complexes: bis(4,7-phenantroline) diperchlorate (Beauchamp & Loeb, 2002), dinitrate (Kopylovich et al., 2001; Barnett et al., 2002), dichloride monohydrate (Malkov et al., 2003) and dibromide (Depree et al., 2000), and one nickel complex, dibromide, has been reported (Assoumatine & Stoeckli-Evans, 2001). All these compounds have 1:2 composition. For a description of the Cambridge Structural Database, see: Allen (2002).

Experimental

Crystal data

[Co(C₂H₃N)₂(H₂O)₄][CoCl₄]
M_r = 413.83
Orthorhombic, P 2₁ 2₁ 2₁
a = 7.0569 (4) Å
b = 12.3209 (8) Å
c = 17.9698 (12) Å
V = 1562.43 (17) Å³
Z = 4
Mo K radiation
= 2.81 mm^-1
T = 170 (2) K
0.2 × 0.2 × 0.2 mm

Data collection

Kuma KM-4-CCD diffractometer
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ) T_min = 0.52, T_max = 0.57
6778 measured reflections
2619 independent reflections
2386 reflections with I > 2(I)
R_int = 0.027

Refinement

R[F² > 2(F²)] = 0.064
wR(F²) = 0.164
S = 1.03
2619 reflections
145 parameters
H-atom parameters constrained
_max = 3.41 e Å^-3
_min = -0.58 e Å^-3
Absolute structure: Flack (1983), 1006 Friedel pairs
Flack parameter: 0.28 (4)

Table 1
Selected bond lengths (Å)

Co1-O1W	2.085 (5)
Co1-O2W	2.076 (5)
Co1-O3W	2.067 (5)
Co1-O4W	2.088 (5)
Co1-N11	2.093 (6)
Co1-N21	2.106 (6)
Co2-Cl1	2.260 (2)
Co2-Cl2	2.2760 (19)
Co2-Cl3	2.2787 (19)
Co2-Cl4	2.3185 (18)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O1W-H1WACl2ⁱ	0.90	2.34	3.185 (6)	155
O1W-H1WBCl3	0.90	2.40	3.250 (6)	157
O2W-H2WACl4ⁱⁱ	0.90	2.29	3.153 (5)	159
O2W-H2WACl4ⁱⁱ	0.90	2.29	3.153 (5)	159
O3W-H3WACl3ⁱ	0.90	2.34	3.163 (6)	152
O3W-H3WBCl1ⁱⁱⁱ	0.90	2.30	3.191 (6)	169
O4W-H4WACl4^iv	0.90	2.35	3.201 (5)	158
O4W-H4WBCl2^v	0.90	2.36	3.199 (6)	155
Symmetry codes: (i) x+1, y, z; (ii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) $[-x+{\script{3\over 2}}, -y+1, z-{\script{1\over 2}}]$ ; (v) $[-x+{\script{1\over 2}}, -y+1, z-{\script{1\over 2}}]$ .

Data collection: CrysAlis CCD (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]$ ); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Stereochemical Workstation Operation Manual (Siemens, 1989) and Mercury (Macrae et al., 2008); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: KP2200 ).

Acknowledgements

This research was carried out as part of a Polish Ministry of Higher Education and Science project (grant No. NN 204 2716 33).

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.
Assoumatine, T. & Stoeckli-Evans, H. (2001). Acta Cryst. E57, m179-m180.
Barnett, S. A., Blake, A. J., Champness, N. R. & Wilson, C. (2002). Acta Cryst. E58, m444-m446.
Beauchamp, D. A. & Loeb, S. J. (2002). Chem. Eur. J. 8, 5084-5088.
Depree, C. V., Ainscough, E. W., Brodie, A. M., Gainsford, G. J. & Lensink, C. (2000). Acta Cryst. C56, 17-18.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Kopylovich, M. N., Kukushkin, V. Yu., Guedes da Silva, M. F. C., Haukka, M., da Silva, J. J. R. F. & Pombeiro, A. J. L. (2001). J. Chem. Soc. Perkin Trans. 1, pp. 1569-1573.
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.
Malkov, A. E., Fomina, I. G., Sidorov, A. A., Aleksandrov, G. G., Egorov, I. M., Latosh, N. I., Chupakhin, O. N., Rusinov, G. L., Rakitin, Yu. V., Novotortsev, V. M., Ikorskii, V. N., Eremenko, I. L. & Moiseev, I. I. (2003). J. Mol. Struct. 656, 207-224.
Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Siemens (1989). Stereochemical Workstation Operation Manual. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
Stefankiewicz, A. R., Walesa, M., Ciesielski, A., Patroniak, V., Kubicki, M., Hnatejko, Z., Harrowfield, J. M. & Lehn, J.-M. (2008). Eur. J. Inorg. Chem. pp. 2910-2920.

metal-organic compounds