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Volume 69 
Part 7 
Pages m391-m392  
July 2013  

Received 21 May 2013
Accepted 4 June 2013
Online 15 June 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.008 Å
Disorder in main residue
R = 0.061
wR = 0.182
Data-to-parameter ratio = 15.4
Details
Open access

Bis[chloridobis(1,10-phenanthroline)copper(II)] pentacyanidonitrosoferrate(II) dimethylformamide monosolvate

aTaras Shevchenko National University, Department of Chemistry, Volodymyrska str. 64/13, 01601 Kyiv, Ukraine, and bSTC, "Institute for Single Crystals", National Academy of Sciences of Ukraine, Lenina ave. 60, Kharkov 61001, Ukraine
Correspondence e-mail: kozachuk_o@yahoo.com

The title complex [CuCl(C12H8N2)2]2[Fe(CN)5(NO)]·C3H7NO, consists of discrete [Cu(phen)2Cl]+ cations (phen is 1,10-phenanthroline), [Fe(CN)5NO]2- anions and one dimethylformamide (DMF) solvent molecule of crystallization per asymmetric unit. The CuII atom is coordinated by two phenanthroline ligands and one chloride ion in a distorted trigonal-bipyramidal geometry. The dihedral angle between the phen ligands is 77.92 (7)°. The cation charge is balanced by a disordered nitroprusside counter-anion with the FeII atom located on an inversion center with a slightly distorted octahedral coordination geometry. In the crystal, weak C-H...N and C-H...Cl hydrogen bonds connect anions and cations into a two-dimensional network parallel to (100). In addition, [pi]-[pi] stacking interactions are observed with centroid-centroid distances in the range 3.565 (2)-3.760 (3)Å. The dimethylformamide solvent molecule was refined as disordered about an inversion center.

Related literature

For background to the direct synthesis of coordination compounds, see: Buvaylo et al. (2005[Buvaylo, E. A., Kokozay, V. N., Vassilyeva, O. Yu., Skelton, B. W., Jezierska, J., Brunel, L. C. & Ozarowski, A. (2005). Chem. Commun. pp. 4976-4978.]); Makhankova et al. (2002[Makhankova, V. G., Vassilyeva, O. Yu., Kokozay, V. N., Skelton, B. W., Sorace, L. & Gatteschi, D. (2002). J. Chem. Soc. Dalton Trans. pp. 4253-4259.]); Nesterova et al. (2004[Nesterova (Pryma), O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W. & Linert, W. (2004). Inorg. Chem. Commun. 7, 450-454.], 2005[Nesterova, O. V., Lipetskaya, A. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W. & Jezierska, J. (2005). Polyhedron, 24, 1425-1434.], 2008[Nesterova, O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W., Jezierska, J., Linert, W. & Ozarowski, A. (2008). Dalton Trans. pp. 1431-1436.]); Pryma et al. (2003[Pryma, O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W., Shishkin, O. V. & Teplytska, T. S. (2003). Eur. J. Inorg. Chem. pp. 1426-1432.]); Vinogradova et al. (2002[Vinogradova, E. A., Vassilyeva, O. Yu., Kokozay, V. N., Skelton, B. W., Bjernemose, J. K. & Raithby, P. R. (2002). J. Chem. Soc. Dalton Trans. pp. 4248-4252.]); Vassilyeva et al. (1997[Vassilyeva, O. Yu., Kokozay, V. N., Zhukova, N. I. & Kovbasyuk, L. A. (1997). Polyhedron, 16, 263-266.]). For the structures of related complexes, see: Nikitina et al. (2008[Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Goreshnik, E. A. & Jezierska, J. (2008). Polyhedron, 27, 2426-2430.]); Vreshch et al. (2009[Vreshch, O. V., Nesterova, O. V., Kokozay, V. N., Skelton, B. W., Garcia, C. J. G. & Jezierska, J. (2009). Inorg. Chem. Commun. 12, 890-894.]); Onawumi et al. (2010[Onawumi, O. O., Adekunle, F. A., Ibrahim, A. O., Rajasekharan, M. V. & Odunola, O. A. (2010). Synth. React. Inorg. Metal-Org. Nano-Met. Chem. 40, 78-83.]); Sui et al. (2006[Sui, A.-X., Zhu, G. & Tang, Z.-X. (2006). Acta Cryst. E62, m1592-m1594.]); Xiao et al. (2004[Xiao, H.-P., Hu, M.-L. & Li, X.-H. (2004). Acta Cryst. E60, m71-m72.]); Soria et al. (2002[Soria, D. B., Villalba, M. E. C., Piro, O. E. & Aymonino, P. J. (2002). Polyhedron, 21, 1767-1774.]); Shevyakova et al. (2002[Shevyakova, I. Yu., Buravov, L. I., Kushch, L. A., Yagubskii, E. B., Khasanov, S. S., Zorina, L. V., Shibaeva, R. P., Drichko, N. V. & Olejniczak, I. (2002). Russ. J. Coord. Chem. 28, 520-529.]).

[Scheme 1]

Experimental

Crystal data
  • [CuCl(C12H8N2)2]2[Fe(CN)5(NO)]·C3H7NO

  • Mr = 1207.85

  • Triclinic, [P \overline 1]

  • a = 9.9645 (13) Å

  • b = 10.6001 (18) Å

  • c = 12.623 (2) Å

  • [alpha] = 79.585 (14)°

  • [beta] = 84.896 (12)°

  • [gamma] = 82.047 (12)°

  • V = 1295.9 (4) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 1.25 mm-1

  • T = 293 K

  • 0.50 × 0.40 × 0.20 mm

Data collection
  • Oxford Diffraction Xcalibur 3 diffractometer

  • Absorption correction: numerical (CrysAlis PRO; Oxford Diffraction, 2010[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]) Tmin = 0.575, Tmax = 0.789

  • 11289 measured reflections

  • 5647 independent reflections

  • 2685 reflections with I > 2[sigma](I)

  • Rint = 0.041

Refinement
  • R[F2 > 2[sigma](F2)] = 0.061

  • wR(F2) = 0.182

  • S = 0.99

  • 5647 reflections

  • 366 parameters

  • 5 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.73 e Å-3

  • [Delta][rho]min = -0.61 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C12-H12...Cl1i 0.93 2.82 3.701 (6) 159
C23-H23...N6ii 0.93 2.52 3.425 (7) 163
Symmetry codes: (i) -x+1, -y+2, -z; (ii) -x, -y+1, -z+1.

Data collection: CrysAlis PRO (Oxford Diffraction, 2010[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]); 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: LH5620 ).


Acknowledgements

This work was partly supported by the State Fund for Fundamental Researches of Ukraine (project 54.3/005).

References

Buvaylo, E. A., Kokozay, V. N., Vassilyeva, O. Yu., Skelton, B. W., Jezierska, J., Brunel, L. C. & Ozarowski, A. (2005). Chem. Commun. pp. 4976-4978.  [CSD] [CrossRef]
Makhankova, V. G., Vassilyeva, O. Yu., Kokozay, V. N., Skelton, B. W., Sorace, L. & Gatteschi, D. (2002). J. Chem. Soc. Dalton Trans. pp. 4253-4259.  [CSD] [CrossRef]
Nesterova, O. V., Lipetskaya, A. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W. & Jezierska, J. (2005). Polyhedron, 24, 1425-1434.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Nesterova, O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W., Jezierska, J., Linert, W. & Ozarowski, A. (2008). Dalton Trans. pp. 1431-1436.  [CSD] [CrossRef]
Nesterova (Pryma), O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W. & Linert, W. (2004). Inorg. Chem. Commun. 7, 450-454.
Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Goreshnik, E. A. & Jezierska, J. (2008). Polyhedron, 27, 2426-2430.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Onawumi, O. O., Adekunle, F. A., Ibrahim, A. O., Rajasekharan, M. V. & Odunola, O. A. (2010). Synth. React. Inorg. Metal-Org. Nano-Met. Chem. 40, 78-83.  [ChemPort]
Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.
Pryma, O. V., Petrusenko, S. R., Kokozay, V. N., Skelton, B. W., Shishkin, O. V. & Teplytska, T. S. (2003). Eur. J. Inorg. Chem. pp. 1426-1432.  [CSD] [CrossRef]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Shevyakova, I. Yu., Buravov, L. I., Kushch, L. A., Yagubskii, E. B., Khasanov, S. S., Zorina, L. V., Shibaeva, R. P., Drichko, N. V. & Olejniczak, I. (2002). Russ. J. Coord. Chem. 28, 520-529.  [CrossRef]
Soria, D. B., Villalba, M. E. C., Piro, O. E. & Aymonino, P. J. (2002). Polyhedron, 21, 1767-1774.  [Web of Science] [CrossRef] [ChemPort]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Sui, A.-X., Zhu, G. & Tang, Z.-X. (2006). Acta Cryst. E62, m1592-m1594.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]
Vassilyeva, O. Yu., Kokozay, V. N., Zhukova, N. I. & Kovbasyuk, L. A. (1997). Polyhedron, 16, 263-266.  [CrossRef] [ChemPort] [Web of Science]
Vinogradova, E. A., Vassilyeva, O. Yu., Kokozay, V. N., Skelton, B. W., Bjernemose, J. K. & Raithby, P. R. (2002). J. Chem. Soc. Dalton Trans. pp. 4248-4252.  [CSD] [CrossRef]
Vreshch, O. V., Nesterova, O. V., Kokozay, V. N., Skelton, B. W., Garcia, C. J. G. & Jezierska, J. (2009). Inorg. Chem. Commun. 12, 890-894.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Xiao, H.-P., Hu, M.-L. & Li, X.-H. (2004). Acta Cryst. E60, m71-m72.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m391-m392   [ doi:10.1107/S1600536813015547 ]

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