Bis(2,2′-bipyridine){ethyl 4′-[N-(4-carbamoylphen­yl)carbamo­yl]-2,2′-bi­pyridine-4-carboxyl­ate}ruthenium(II) bis­[hexa­fluorido­phosphate(V)]

Hirahara, M.; Masaoka, S.; Sakai, K.

doi:10.1107/S1600536809002360

Volume 65
Part 2
Pages m228-m229
February 2009

Received 19 November 2008
Accepted 19 January 2009
Online 28 January 2009

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.005 Å
R = 0.043
wR = 0.113
Data-to-parameter ratio = 15.2
Details

Bis(2,2'-bipyridine){ethyl 4'-[N-(4-carbamoylphenyl)carbamoyl]-2,2'-bipyridine-4-carboxylate}ruthenium(II) bis[hexafluoridophosphate(V)]

Masanari Hirahara,^a Shigeyuki Masaoka ^a and Ken Sakai ^a ^*

^aDepartment of Chemistry, Faculty of Science, Kyushu University, Hakozaki 6-10-1, Higashi-ku, Fukuoka 812-8581, Japan
Correspondence e-mail: ksakai@chem.kyushu-univ.jp

In the title compound, [Ru(C₁₀H₈N₂)₂(C₂₁H₁₈N₄O₄)](PF₆)₂, the Ru^II complex cation reveals a slightly distorted octahedral coordination. The coordination bonds of the 4,4'-substituted bipyridyl donors [Ru-N = 2.038 (3) and 2.051 (3) Å] are shorter than those of the 2,2'-bipyridyl donors [Ru-N1 = 2.065 (3)-2.077 (3) Å], due to the electron-withdrawing effects of the substituents at the 4,4'-positions. The angles between the pyridyl planes of the three bipyridyl ligands are 1.5 (2), 6.3 (3) and 8.7 (2)°, respectively. The cations are connected by anions via N-HF interactions.

Related literature

For related literature, see: Gillaizeau-Gauthier et al. (2001); Ozawa & Sakai (2007); Ozawa et al. (2006, 2007); Sakai & Ozawa (2007); Sakai et al. (1993). For discussion of attractive interactions between negatively-charged atoms and alpha C atoms from heterocyclic rings, see: Schottel et al. (2008).

Experimental

Crystal data

[Ru(C₁₀H₈N₂)₂(C₂₁H₁₈N₄O₄)](PF₆)₂
M_r = 1093.77
Monoclinic, P 2₁ /c
a = 18.400 (3) Å
b = 13.187 (2) Å
c = 18.863 (3) Å
= 111.344 (2)°
V = 4262.9 (11) Å³
Z = 4
Mo K radiation
= 0.55 mm^-1
T = 100 (s.u.?) K
0.20 × 0.10 × 0.03 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.717, T_max = 0.986
23329 measured reflections
9357 independent reflections
6405 reflections with I > 2(I)
R_int = 0.047

Refinement

R[F² > 2(F²)] = 0.043
wR(F²) = 0.113
S = 1.00
9357 reflections
614 parameters
H-atom parameters constrained
_max = 0.79 e Å^-3
_min = -0.48 e Å^-3

Table 1
Selected bond lengths (Å)

Ru1-N1	2.077 (3)
Ru1-N2	2.070 (3)
Ru1-N3	2.076 (3)
Ru1-N4	2.065 (3)
Ru1-N5	2.051 (3)
Ru1-N6	2.038 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N7-H7F2ⁱ	0.86	2.34	3.181 (4)	168
N8-H8BF10ⁱ	0.86	2.29	2.999 (5)	139
Symmetry code: (i) $[x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2006); cell refinement: APEX2; data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: KENX (Sakai, 2004); software used to prepare material for publication: SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEPII (Johnson, 1976).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: KP2198 ).

Acknowledgements

This work was in part supported by a Grant-in-Aid for Scientific Research (A) (No. 17205008), a Grant-in-Aid for Specially Promoted Research (No. 18002016), and a Grant-in-Aid for the Global COE Program (`Science for Future Molecular Systems') from the Ministry of Education, Culture, Sports, Science and Technology of Japan.

References

Bruker (2004). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2006). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Gillaizeau-Gauthier, I., Odobel, F., Alebbi, M., Argazzi, R., Costa, E., Bignozzi, C. A., Qu, P. & Meyer, G. J. (2001). Inorg. Chem. 40, 6073-6079.
Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA.
Molecular Structure Corporation (2001). TEXSAN. MSC, The Woodlands, Texas, USA.
Ozawa, H., Haga, M. & Sakai, K. (2006). J. Am. Chem. Soc. 128, 4926-4927.
Ozawa, H. & Sakai, K. (2007). Chem. Lett. 36, 920-921.
Ozawa, H., Yokoyama, Y., Haga, M. & Sakai, K. (2007). Dalton Trans. pp. 1197-1206.
Sakai, K. (2004). KENX. Kyushu University, Japan.
Sakai, K., Kizaki, Y., Tsubomura, T. & Matumoto, K. (1993). J. Mol. Catal. 79, 141-152.
Sakai, K. & Ozawa, H. (2007). Coord. Chem. Rev. 251, 2753-2766.
Schottel, B. L., Chifotides, H. T. & Dunbar, K. R. (2008). Chem. Soc. Rev. 37, 68-83.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds