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Volume 68 
Part 5 
Pages m531-m532  
May 2012  

Received 15 March 2012
Accepted 24 March 2012
Online 4 April 2012

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Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.007 Å
R = 0.051
wR = 0.135
Data-to-parameter ratio = 15.9
Details
Open access

Tris(1,10-phenanthroline-[kappa]2N,N')iron(II) bis[(1,10-phenanthroline-[kappa]2N,N')tetrakis(thiocyanato-[kappa]N)chromate(III)] acetonitrile trisolvate monohydrate

Valentyna V. Semenaka,a* Oksana V. Nesterova,a Volodymyr N. Kokozaya and Volodymyr V. Bonb

aDepartment of Inorganic Chemistry, Taras Shevchenko National University of Kyiv, 64 Volodymyrs'ka St., Kyiv 01601, Ukraine, and bDepartment of Chemistry of Complex Compounds, V.I. Vernadsky Institute of General and Inorganic Chemistry, National Academy of Sciences of Ukraine, 32/34 Palladin Ave., Kyiv 03680, Ukraine
Correspondence e-mail: valya.semenaka@gmail.com

Single crystals of the title heterometallic compound, [Fe(C12H8N2)3][Cr(NCS)4(C12H8N2)]2·3CH3CN·H2O or [Fe(Cphen)3][Cr(NCS)4(phen)]2·3CH3CN·H2O, were prepared using the one-pot open-air reaction of iron powder, Reineckes salt and 1,10-phenanthroline (phen) in acetonitrile. The asymetric unit consists of an [Fe(phen)3]2+ cation, two [Cr(phen)(NCS)4]- anions, three acetonitrile solvent molecules and a water molecule. The Fe and Cr atoms both show a slightly distorted octahedral FeN6 and CrN6 coordination geometry with adjacent angles in the range 79.67 (12)-95.21 (12)°. No classical hydrogen bonding involving the water molecule is observed.

Related literature

For background to direct synthesis, see: Makhankova (2011[Makhankova, V. G. (2011). Glob. J. Inorg. Chem. 2, 265-285.]). For background to the use of Reineckes salt as a source of building blocks or metalloligands, see: Zhang et al. (2001[Zhang, K.-L., Chen, W., Xu, Y., Wang, Z., Zhong, Z. J. & You, X.-Z. (2001). Polyhedron, 20, 2033-2036.]); Cucos et al. (2006[Cucos, A., Avarvari, N., Andruh, M., Journaux, Y., Muller, A. & Schmidtmann, M. (2006). Eur. J. Inorg. Chem. pp. 903-907.]); Cherkasova & Gorunova (2003[Cherkasova, T. G. & Gorunova, I. P. (2003). Zh. Neorg. Khim. 48, 611-615.]); Nikitina et al. (2009[Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Dyakonenko, V. V., Shishkin, O. V. & Jezierska, J. (2009). Polyhedron, 28, 1265-1272.]); Kolotilov et al. (2010[Kolotilov, S. V., Cador, O., Gavrilenko, K. S., Golhen, S., Ouahab, L. & Pavlishchuk, V. V. (2010). Eur. J. Inorg. Chem. 8, 1255-1266.]). For Fe-N bond lengths in iron-phen derivatives, see: Alonso et al. (2005[Alonso, C., Ballster, L., Gutierrez, F., Rerpinaqn, M. F., Sanchez, A. E. & Azcondo, M. T. (2005). Eur. J. Inorg. Chem. pp. 486-495.]). For a related structure, see: Semenaka et al. (2011[Semenaka, V. V., Nesterova, O. V., Kokozay, V. N., Zybatyuk, R. I. & Shishkin, O. V. (2011). Acta Cryst. E67, m1021-m1022.]).

[Scheme 1]

Experimental

Crystal data

  • [Fe(C12H8N2)3][Cr(NCS)4(C12H8N2)]2·3C2H3N·H2O

  • Mr = 1666.69

  • Triclinic, [P \overline 1]

  • a = 12.641 (2) Å

  • b = 16.681 (3) Å

  • c = 20.692 (4) Å

  • [alpha] = 111.514 (5)°

  • [beta] = 107.291 (6)°

  • [gamma] = 92.231 (5)°

  • V = 3821.5 (13) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.75 mm-1

  • T = 173 K

  • 0.23 × 0.22 × 0.12 mm
Data collection

  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS.. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.847, Tmax = 0.916

  • 48046 measured reflections

  • 15519 independent reflections

  • 8993 reflections with I > 2[sigma](I)

  • Rint = 0.078
Refinement

  • R[F2 > 2[sigma](F2)] = 0.051

  • wR(F2) = 0.135

  • S = 0.99

  • 15519 reflections

  • 974 parameters

  • 3 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.43 e Å-3

  • [Delta][rho]min = -0.44 e Å-3

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS.. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS.. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: 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: RU2031 ).

References

Alonso, C., Ballster, L., Gutierrez, F., Rerpinaqn, M. F., Sanchez, A. E. & Azcondo, M. T. (2005). Eur. J. Inorg. Chem. pp. 486-495.  [ISI] [CSD] [CrossRef]
Bruker (2005). APEX2, SAINT and SADABS.. Bruker AXS Inc., Madison, Wisconsin, USA.
Cherkasova, T. G. & Gorunova, I. P. (2003). Zh. Neorg. Khim. 48, 611-615.  [ChemPort]
Cucos, A., Avarvari, N., Andruh, M., Journaux, Y., Muller, A. & Schmidtmann, M. (2006). Eur. J. Inorg. Chem. pp. 903-907.  [ISI] [CSD] [CrossRef]
Kolotilov, S. V., Cador, O., Gavrilenko, K. S., Golhen, S., Ouahab, L. & Pavlishchuk, V. V. (2010). Eur. J. Inorg. Chem. 8, 1255-1266.  [ISI] [CrossRef]
Makhankova, V. G. (2011). Glob. J. Inorg. Chem. 2, 265-285.  [ChemPort]
Nikitina, V. M., Nesterova, O. V., Kokozay, V. N., Dyakonenko, V. V., Shishkin, O. V. & Jezierska, J. (2009). Polyhedron, 28, 1265-1272.  [ISI] [CSD] [CrossRef] [ChemPort]
Semenaka, V. V., Nesterova, O. V., Kokozay, V. N., Zybatyuk, R. I. & Shishkin, O. V. (2011). Acta Cryst. E67, m1021-m1022.  [CrossRef] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [ISI] [CrossRef] [details]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]
Zhang, K.-L., Chen, W., Xu, Y., Wang, Z., Zhong, Z. J. & You, X.-Z. (2001). Polyhedron, 20, 2033-2036.  [ISI] [CSD] [CrossRef] [ChemPort]

Acta Cryst (2012). E68, m531-m532   [ doi:10.1107/S1600536812012949 ]

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