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Volume 68 
Part 12 
Pages m1570-m1571  
December 2012  

Received 14 November 2012
Accepted 26 November 2012
Online 30 November 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.010 Å
Disorder in solvent or counterion
R = 0.071
wR = 0.218
Data-to-parameter ratio = 12.6
Details
Open access

Tris(1,10-phenanthroline-[kappa]2N,N')ruthenium(II) bis(perchlorate)

aInstitute of Chemistry, University of Bialystok, Hurtowa 1, 15-399 Bialystok, Poland
Correspondence e-mail: k.brzezinski@uwb.edu.pl

The asymmetric unit of the title compound, [Ru(C12H8N2)3](ClO4)2, contains one octahedrally coordinated RuII cation of the ruthenium-phenanthroline complex and three differently occupied perchlorate anions: two, denoted A and B, are located on the twofold axis while another, denoted C, is positioned in the proximity of the twofold screw axis. Perchlorate anions B and C are severely disordered. The occupancies of the two major conformers of anion B refined to 0.302 (6) and 0.198 (6). Perchlorate ion C was modeled in two alternate conformations which refined to occupancies of 0.552 (10) and 0.448 (10).

Related literature

For the preparation of phenanthroline complexes with transition metals, see: Burstall & Nyholm (1952[Burstall, F. H. & Nyholm, R. S. (1952). J. Chem. Soc. pp. 3570-3579.]). For the structures of salts of complexes of ruthenium with phenanthroline, see: Breu & Stoll (1996[Breu, J. & Stoll, A. J. (1996). Acta Cryst. C52, 1174-1177.]); Maloney & MacDonnell (1997[Maloney, D. J. & MacDonnell, F. M. (1997). Acta Cryst. C53, 705-707.]); Otsuka et al. (2001[Otsuka, T., Sekine, A., Fujigasaki, N., Ohashi, Y. & Kaizu, Y. (2001). Inorg. Chem. 40, 3406-3412.]); Wu et al. (2001[Wu, J. Z., Zhou, Z.-Y. & Ji, L. N. (2001). Cryst. Res. Technol. 36, 101-105.]); Ghazzali et al. (2008[Ghazzali, M., Öhrström, L., Lincoln, P. & Langer, V. (2008). Acta Cryst. C64, m243-m245.]). For background to the properties and applications of phenanthroline complexes, see: Juris et al. (1988[Juris, A., Balzani, V., Barigelletti, F., Campagna, S., Belser, P. & von Zalewsky, A. (1988). Coord. Chem. Rev. 84, 85-99.]); D'Angelantonio et al. (1991[D'Angelantonio, M., Mulazzani, Q. G., Venturi, M., Ciano, M. & Hoffman, M. Z. (1991). J. Phys. Chem. 95, 5121-5129.]); Balzani et al. (1996[Balzani, V., Juris, A., Venturi, M., Campagna, S. & Serroni, S. (1996). Chem. Rev. 96, 759-772.]); Mills & Williams (1997[Mills, A. & Williams, F. C. (1997). Thin Solid Films, 306, 163-170.]); Yang et al. (1997[Yang, G., Wu, J. Z., Wang, L., Ji, L. N. & Tian, X. (1997). J. Inorg. Biochem. 66, 141-144.]); Miyasaka et al. (2001[Miyasaka, H., Clearc, R., Campos-Fernandez, C. S. & Dunbar, K. R. (2001). Inorg. Chem. 40, 1663-1669.]); Plonska et al. (2002[Plonska, M. E., Dubis, A. & Winkler, K. (2002). J. Electroanal. Chem. 526, 77-84.]); Winkler et al. (2006[Winkler, K., Plonska, M. E., Recko, K. & Dobrzynski, L. (2006). Electrochim. Acta, 51, 4544-4553.]).

[Scheme 1]

Experimental

Crystal data
  • [Ru(C12H8N2)3](ClO4)2

  • Mr = 840.57

  • Monoclinic, C 2/c

  • a = 35.408 (7) Å

  • b = 16.106 (3) Å

  • c = 12.056 (2) Å

  • [beta] = 102.22 (3)°

  • V = 6720 (2) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 0.69 mm-1

  • T = 100 K

  • 0.22 × 0.19 × 0.10 mm

Data collection
  • Agilent SuperNova (Dual, Cu at zero, Atlas) diffractometer

  • Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011[Agilent (2011). CrysAlis PRO. Agilent Technologies, Yarnton, England.]) Tmin = 0.859, Tmax = 1.000

  • 28067 measured reflections

  • 6867 independent reflections

  • 5365 reflections with I > 2[sigma](I)

  • Rint = 0.039

Refinement
  • R[F2 > 2[sigma](F2)] = 0.071

  • wR(F2) = 0.218

  • S = 1.04

  • 6867 reflections

  • 545 parameters

  • 181 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 2.55 e Å-3

  • [Delta][rho]min = -1.22 e Å-3

Data collection: CrysAlis PRO (Agilent, 2011[Agilent (2011). CrysAlis PRO. Agilent Technologies, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXD (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 2012)[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]; software used to prepare material for publication: SHELXL97.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BX2430 ).


Acknowledgements

This work was supported by the HOMING PLUS project of the Foundation for Polish Science (MK and PR). The X-ray diffractometer was funded by the EFRD as part of the Operational Programme Development of Eastern Poland 2007-2013, project: POPW.01.03.00-20-034/09-00.

References

Agilent (2011). CrysAlis PRO. Agilent Technologies, Yarnton, England.
Balzani, V., Juris, A., Venturi, M., Campagna, S. & Serroni, S. (1996). Chem. Rev. 96, 759-772.  [CrossRef] [PubMed] [ChemPort]
Breu, J. & Stoll, A. J. (1996). Acta Cryst. C52, 1174-1177.  [CSD] [CrossRef] [details]
Burstall, F. H. & Nyholm, R. S. (1952). J. Chem. Soc. pp. 3570-3579.  [CrossRef]
D'Angelantonio, M., Mulazzani, Q. G., Venturi, M., Ciano, M. & Hoffman, M. Z. (1991). J. Phys. Chem. 95, 5121-5129.  [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Ghazzali, M., Öhrström, L., Lincoln, P. & Langer, V. (2008). Acta Cryst. C64, m243-m245.  [CrossRef] [details]
Juris, A., Balzani, V., Barigelletti, F., Campagna, S., Belser, P. & von Zalewsky, A. (1988). Coord. Chem. Rev. 84, 85-99.  [CrossRef] [ChemPort]
Maloney, D. J. & MacDonnell, F. M. (1997). Acta Cryst. C53, 705-707.  [CSD] [CrossRef] [details]
Mills, A. & Williams, F. C. (1997). Thin Solid Films, 306, 163-170.  [CrossRef] [ChemPort]
Miyasaka, H., Clearc, R., Campos-Fernandez, C. S. & Dunbar, K. R. (2001). Inorg. Chem. 40, 1663-1669.  [CrossRef] [PubMed] [ChemPort]
Otsuka, T., Sekine, A., Fujigasaki, N., Ohashi, Y. & Kaizu, Y. (2001). Inorg. Chem. 40, 3406-3412.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Plonska, M. E., Dubis, A. & Winkler, K. (2002). J. Electroanal. Chem. 526, 77-84.  [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Winkler, K., Plonska, M. E., Recko, K. & Dobrzynski, L. (2006). Electrochim. Acta, 51, 4544-4553.  [ISI] [CrossRef] [ChemPort]
Wu, J. Z., Zhou, Z.-Y. & Ji, L. N. (2001). Cryst. Res. Technol. 36, 101-105.  [CrossRef] [ChemPort]
Yang, G., Wu, J. Z., Wang, L., Ji, L. N. & Tian, X. (1997). J. Inorg. Biochem. 66, 141-144.  [CrossRef] [ChemPort] [PubMed]


Acta Cryst (2012). E68, m1570-m1571   [ doi:10.1107/S1600536812048428 ]

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