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Volume 69 
Part 1 
Pages m1-m2  
January 2013  

Received 15 November 2012
Accepted 24 November 2012
Online 5 December 2012

Key indicators
Single-crystal X-ray study
T = 93 K
Mean [sigma](C-C) = 0.005 Å
Disorder in main residue
R = 0.032
wR = 0.062
Data-to-parameter ratio = 15.7
Details
Open access

cis-Bis(2,2'-bipyridine-[kappa]2N,N')carbonylchloridoruthenium(II) hexafluoridophosphate

aCenter for Practical and Project-Based Learning, Cluster of Science and Technology, Fukushima University, 1 Kanayagawa, Fukushima 960-1296, Japan,bDepartment of Materials Science, Graduate School of Science and Technology, Fukushima University, 1 Kanayagawa, Fukushima 960-1296, Japan, and cDepartment of Industrial Systems Engineering, Cluster of Science and Technology, Fukushima University, 1 Kanayagawa, Fukushima 960-1296, Japan
Correspondence e-mail: daio@sss.fukushima-u.ac.jp

In the title compound, [RuCl(C10H8N2)2(CO)]PF6, the RuII atom is coordinated in a distorted octahedral geometry by four N atoms of the bipyridine ligands, a carbonyl C atom and a chloride ion. The carbonyl and chloride ligands in the cation adopt a mutually cis arrangement and these are disordered over two sets of sites with site occupancies of 0.721 (6) and 0.279 (6). The Ru-N bond length [2.117 (2) Å] trans to the carbonyl ligand is slightly longer than the average of the other Ru-N bond lengths (2.08 Å), which can be explained by the expected trans influence of the carbonyl group. In the crystal, weak C-H...F interactions are observed between the complex cation and the PF6- anion, leading to the formation of a three-dimensional supramolecular structure. The crystal studied was an inversion twin with twin fractions of 0.78 (4) and 0.22 (4).

Related literature

For details of the synthesis, see: Oyama et al. (2012[Oyama, D., Suzuki, K., Yamanaka, T. & Takase, T. (2012). J. Coord. Chem. 65, 78-86.]). For a related structure, see: Clear et al. (1980[Clear, J. M., Kelly, J. M. O., Connell, C. M., Vos, J. G., Cardin, C. J., Costa, S. R. & Edwards, A. J. (1980). J. Chem. Soc. Chem. Commun. pp. 750-751.]). For general background to catalytic reactions using [Ru(bpy)2(CO)Cl]+, see: Ishida et al. (1986[Ishida, H., Tanaka, K., Morimoto, M. & Tanaka, T. (1986). Organometallics, 5, 724-730.]); Lehn & Ziessel (1990[Lehn, J.-M. & Ziessel, R. (1990). J. Organomet. Chem. 382, 157-173.]).

[Scheme 1]

Experimental

Crystal data
  • [RuCl(C10H8N2)2(CO)]·PF6

  • Mr = 621.87

  • Orthorhombic, P 21 21 21

  • a = 10.882 (5) Å

  • b = 12.063 (5) Å

  • c = 17.410 (7) Å

  • V = 2285.2 (17) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.95 mm-1

  • T = 93 K

  • 0.20 × 0.10 × 0.02 mm

Data collection
  • Rigaku Saturn diffractometer

  • Absorption correction: multi-scan (REQAB; Jacobson, 1998[Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.897, Tmax = 0.981

  • 22875 measured reflections

  • 5177 independent reflections

  • 4689 reflections with F2 > 2[sigma](F2)

  • Rint = 0.045

Refinement
  • R[F2 > 2[sigma](F2)] = 0.032

  • wR(F2) = 0.062

  • S = 1.08

  • 5177 reflections

  • 330 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.37 e Å-3

  • [Delta][rho]min = -1.28 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 2249 Friedel pairs

  • Flack parameter: 0.22 (4)

Table 1
Selected bond lengths (Å)

Ru1-Cl1 2.3521 (17)
Ru1-N1 2.086 (2)
Ru1-N2 2.070 (2)
Ru1-N3 2.070 (2)
Ru1-N4 2.117 (2)
Ru1-C21 1.890 (8)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C3-H3...F2i 0.95 2.46 3.166 (4) 131
C4-H4...F1ii 0.95 2.41 3.257 (4) 148
C7-H5...F1ii 0.95 2.54 3.431 (4) 156
C8-H6...F2iii 0.95 2.50 3.265 (4) 138
C13-H11...F5iv 0.95 2.39 3.331 (4) 168
Symmetry codes: (i) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) [-x+{\script{1\over 2}}, -y+1, z-{\script{1\over 2}}]; (iii) [x-{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]; (iv) [x-{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1].

Data collection: CrystalClear-SM (Rigaku, 2009[Rigaku (2009). CrystalClear-SM. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear-SM; data reduction: CrystalClear-SM; program(s) used to solve structure: SIR97 (Altomare et al., 1999[Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: CrystalStructure (Rigaku, 2006[Rigaku (2006). CrystalStructure. Rigaku Corporation, Tokyo, Japan.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS5220 ).


References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.  [ISI] [CrossRef] [ChemPort] [details]
Clear, J. M., Kelly, J. M. O., Connell, C. M., Vos, J. G., Cardin, C. J., Costa, S. R. & Edwards, A. J. (1980). J. Chem. Soc. Chem. Commun. pp. 750-751.  [CrossRef] [ISI]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Ishida, H., Tanaka, K., Morimoto, M. & Tanaka, T. (1986). Organometallics, 5, 724-730.  [CrossRef] [ChemPort]
Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.
Lehn, J.-M. & Ziessel, R. (1990). J. Organomet. Chem. 382, 157-173.  [CrossRef] [ChemPort]
Oyama, D., Suzuki, K., Yamanaka, T. & Takase, T. (2012). J. Coord. Chem. 65, 78-86.  [ISI] [CSD] [CrossRef] [ChemPort]
Rigaku (2006). CrystalStructure. Rigaku Corporation, Tokyo, Japan.
Rigaku (2009). CrystalClear-SM. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2013). E69, m1-m2   [ doi:10.1107/S1600536812048246 ]

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