Tris(1,10-phenanthroline-κ2N,N′)ruthenium(II) bis­(perchlorate)

Kozlowska, M.; Rodziewicz, P.; Brus, D.M.; Czyrko, J.; Brzezinski, K.

doi:10.1107/S1600536812048428

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 (C-C) = 0.010 Å
Disorder in solvent or counterion
R = 0.071
wR = 0.218
Data-to-parameter ratio = 12.6
Details

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

Mariana Kozlowska,^a Pawel Rodziewicz,^a Diana Malgorzata Brus,^a Justyna Czyrko ^a and Krzysztof Brzezinski ^a ^*

^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 Ru^II 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). For the structures of salts of complexes of ruthenium with phenanthroline, see: Breu & Stoll (1996); Maloney & MacDonnell (1997); Otsuka et al. (2001); Wu et al. (2001); Ghazzali et al. (2008). For background to the properties and applications of phenanthroline complexes, see: Juris et al. (1988); D'Angelantonio et al. (1991); Balzani et al. (1996); Mills & Williams (1997); Yang et al. (1997); Miyasaka et al. (2001); Plonska et al. (2002); Winkler et al. (2006).

Experimental

Crystal data

[Ru(C₁₂H₈N₂)₃](ClO₄)₂
M_r = 840.57
Monoclinic, C 2/c
a = 35.408 (7) Å
b = 16.106 (3) Å
c = 12.056 (2) Å
= 102.22 (3)°
V = 6720 (2) Å³
Z = 8
Mo K radiation
= 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) T_min = 0.859, T_max = 1.000
28067 measured reflections
6867 independent reflections
5365 reflections with I > 2(I)
R_int = 0.039

Refinement

R[F² > 2(F²)] = 0.071
wR(F²) = 0.218
S = 1.04
6867 reflections
545 parameters
181 restraints
H-atom parameters constrained
_max = 2.55 e Å^-3
_min = -1.22 e Å^-3

Data collection: CrysAlis PRO (Agilent, 2011); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXD (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 2012); 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

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