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Volume 69 
Part 12 
Pages m684-m685  
December 2013  

Received 5 November 2013
Accepted 21 November 2013
Online 27 November 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.006 Å
Disorder in main residue
R = 0.050
wR = 0.109
Data-to-parameter ratio = 13.6
Details
Open access

Bis(2,9-dimethyl-1,10-phenanthroline)copper(I) penta­cyanido­nitro­soferrate(II)

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

The asymmetric unit of the title complex [Cu(C14H12N2)2]2[Fe(CN)5(NO)], consists of a [Cu(dmp)2]+ cation (dmp is 2,9-dimethyl-1,10-phenanthroline) and half an [Fe(CN)5(NO)]2- anion. The anion is disordered across an inversion center with the FeII ion slightly offset (ca 0.205Å) from the inversion center in the direction of the disordered trans-coordinating CN/NO ligands. The anion has a distorted octa­hedral coordination geometry. The CuI ion is coordinated by two phenanthroline ligands in a distorted tetra­hedral geometry. The dihedral angle between the phenanthroline ligands is 77.16 (4) Å. In the crystal, the cations are connected to the anions by weak C-H...N hydrogen bonds. In addition, weak [pi]-[pi] stacking inter­actions are observed, with centroid-centroid distances in the range 3.512 (3)-3.859 (3) Å.

Related literature

For background to the direct synthesis of coordination compounds, see: Kokozay & Vassilyeva (2002[Kokozay, V. N. & Vassilyeva, O. Yu. (2002). Transition Met. Chem. 27, 693-699.]); Nesterova et al. (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.]). For the direct synthesis of heterometallic Cu-containing complexes, 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.]); 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.]); 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.]). For the application of anionic complexes in the preparation of heterometallic compounds, see: Nikitina et al. (2008[Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Goreshnik, E. A. & Jezierska, J. (2008). Polyhedron, 27, 2426-2430.], 2009[Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Dyakonenko, V. V., Shishkin, O. V. & Jezierska, J. (2009). Inorg. Chem. Commun. 12, 101-104.]). For the structures of related complexes, see: Blake et al. (1998[Blake, A. J., Hill, S. J., Hubberstey, P. & Li, W. S. (1998). J. Chem. Soc. Dalton Trans. pp. 909-915.]); Chen et al. (2002[Chen, L. X., Jenning, G., Liu, T., Gosztola, D. J., Hessler, J. P., Scaltrito, D. V. & Meyers, G. J. (2002). J. Am. Chem. Soc. 124, 10861-10867.]); Morpurgo et al. (1984[Morpurgo, G., Dessy, G. & Fares, V. (1984). J. Chem. Soc. Dalton Trans. pp. 785-791.]); Cuttell et al. (2002[Cuttell, D. G., Kuang, S. M., Fanwick, P. E., McMillin, D. R. & Walton, R. A. (2002). J. Am. Chem. Soc. 124, 6-7.]); King et al. (2005[King, G., Gembicky, M. & Coppens, P. (2005). Acta Cryst. C61, m329-m332.]); 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.]); Peresyp­kina & Vostrikova (2012[Peresypkina, E. V. & Vostrikova, K. E. (2012). Dalton Trans. 41, 4100-4106.]).

[Scheme 1]

Experimental

Crystal data
  • [Cu(C14H12N2)2]2[Fe(CN)5(NO)]

  • Mr = 1176.06

  • Triclinic, [P \overline 1]

  • a = 7.371 (3) Å

  • b = 13.741 (3) Å

  • c = 15.065 (4) Å

  • [alpha] = 115.269 (4)°

  • [beta] = 95.327 (3)°

  • [gamma] = 101.323 (4)°

  • V = 1325.9 (7) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 1.12 mm-1

  • T = 293 K

  • 0.50 × 0.40 × 0.20 mm

Data collection
  • Oxford Diffraction Xcalibur3 diffractometer

  • Absorption correction: numerical (CrysAlis PRO; Oxford Diffraction, 2010[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]) Tmin = 0.604, Tmax = 0.807

  • 8613 measured reflections

  • 5112 independent reflections

  • 3100 reflections with I > 2[sigma](I)

  • Rint = 0.048

Refinement
  • R[F2 > 2[sigma](F2)] = 0.050

  • wR(F2) = 0.109

  • S = 0.93

  • 5112 reflections

  • 377 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.38 e Å-3

  • [Delta][rho]min = -0.31 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C17-H17...N6i 0.93 2.55 3.393 (6) 151
Symmetry code: (i) -x+2, -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; 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: LH5667 ).


Acknowledgements

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

References

Blake, A. J., Hill, S. J., Hubberstey, P. & Li, W. S. (1998). J. Chem. Soc. Dalton Trans. pp. 909-915.  [CSD] [CrossRef]
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]
Chen, L. X., Jenning, G., Liu, T., Gosztola, D. J., Hessler, J. P., Scaltrito, D. V. & Meyers, G. J. (2002). J. Am. Chem. Soc. 124, 10861-10867.  [Web of Science] [CrossRef] [PubMed] [ChemPort]
Cuttell, D. G., Kuang, S. M., Fanwick, P. E., McMillin, D. R. & Walton, R. A. (2002). J. Am. Chem. Soc. 124, 6-7.  [Web of Science] [CSD] [CrossRef] [PubMed] [ChemPort]
King, G., Gembicky, M. & Coppens, P. (2005). Acta Cryst. C61, m329-m332.  [CSD] [CrossRef] [IUCr Journals]
Kokozay, V. N. & Vassilyeva, O. Yu. (2002). Transition Met. Chem. 27, 693-699.  [Web of Science] [CrossRef] [ChemPort]
Morpurgo, G., Dessy, G. & Fares, V. (1984). J. Chem. Soc. Dalton Trans. pp. 785-791.  [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., Dyakonenko, V. V., Shishkin, O. V. & Jezierska, J. (2009). Inorg. Chem. Commun. 12, 101-104.  [Web of Science] [CSD] [CrossRef] [ChemPort]
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]
Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.
Peresypkina, E. V. & Vostrikova, K. E. (2012). Dalton Trans. 41, 4100-4106.  [CSD] [CrossRef] [ChemPort] [PubMed]
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]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m684-m685   [ doi:10.1107/S1600536813031760 ]

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