cis-Bis(2,2′-bipyridine-κ2N,N′)carbonyl­chloridoruthenium(II) hexa­fluorido­phosphate

Takase, T.; Mun, B.; Oyama, D.

doi:10.1107/S1600536812048246

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 (C-C) = 0.005 Å
Disorder in main residue
R = 0.032
wR = 0.062
Data-to-parameter ratio = 15.7
Details

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

Tsugiko Takase,^a Bisa Mun ^b and Dai Oyama ^c ^*

^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 Ru^II 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-HF 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). For a related structure, see: Clear et al. (1980). For general background to catalytic reactions using [Ru(bpy)₂(CO)Cl]⁺, see: Ishida et al. (1986); Lehn & Ziessel (1990).

Experimental

Crystal data

[RuCl(C₁₀H₈N₂)₂(CO)]·PF₆
M_r = 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 radiation
= 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) T_min = 0.897, T_max = 0.981
22875 measured reflections
5177 independent reflections
4689 reflections with F² > 2(F²)
R_int = 0.045

Refinement

R[F² > 2(F²)] = 0.032
wR(F²) = 0.062
S = 1.08
5177 reflections
330 parameters
H-atom parameters constrained
_max = 1.37 e Å^-3
_min = -1.28 e Å^-3
Absolute structure: Flack (1983), 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-HA	D-H	HA	DA	D-HA
C3-H3F2ⁱ	0.95	2.46	3.166 (4)	131
C4-H4F1ⁱⁱ	0.95	2.41	3.257 (4)	148
C7-H5F1ⁱⁱ	0.95	2.54	3.431 (4)	156
C8-H6F2ⁱⁱⁱ	0.95	2.50	3.265 (4)	138
C13-H11F5^iv	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); cell refinement: CrystalClear-SM; data reduction: CrystalClear-SM; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: CrystalStructure (Rigaku, 2006).

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.
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.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Ishida, H., Tanaka, K., Morimoto, M. & Tanaka, T. (1986). Organometallics, 5, 724-730.
Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.
Lehn, J.-M. & Ziessel, R. (1990). J. Organomet. Chem. 382, 157-173.
Oyama, D., Suzuki, K., Yamanaka, T. & Takase, T. (2012). J. Coord. Chem. 65, 78-86.
Rigaku (2006). CrystalStructure. Rigaku Corporation, Tokyo, Japan.
Rigaku (2009). CrystalClear-SM. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds

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