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Volume 68 
Part 1 
Pages m77-m78  
January 2012  

Received 12 December 2011
Accepted 16 December 2011
Online 23 December 2011

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Key indicators
Single-crystal X-ray study
T = 180 K
Mean [sigma](C-C) = 0.006 Å
Disorder in solvent or counterion
R = 0.040
wR = 0.112
Data-to-parameter ratio = 12.9
Details
Open access

(2,2'-Bipyridine-4,4'-dicarboxylic acid-[kappa]2N,N')chlorido(2,2':6',2''-terpyridyl-[kappa]3N,N',N'')ruthenium(II) perchlorate ethanol monosolvate monohydrate

Anne Nielsen,a Christine J. McKenziea and Andrew D. Bonda*

aUniversity of Southern Denmark, Department of Physics and Chemistry, Campusvej 55, 5230 Odense, Denmark
Correspondence e-mail: adb@chem.sdu.dk

In the title compound, [RuCl(C15H11N3)(C12H8N2O4)]ClO4·C2H5OH·H2O, the geometry of the ClN5 coordination set around the RuII atom is close to octahedral, but distorted on account of the limited bite angles of the polypyridyl ligands. The complexes are linked by O-H...O hydrogen bonds between the carboxyl groups and the crystal lattice water molecules into chains along [110]. Face-to-face stacking interactions are formed between terpyridine ligands, with interplanar separations of 3.66 (1) and 3.42 (1) Å, and between bipyridine-4,4'-dicarboxylic acid ligands, with interplanar separations of 3.65 (1) and 3.72 (1) Å. Three O atoms of the perchlorate ion are each disordered equally over two positions. The hydroxy group of the ethanol molecule is also disordered over two sites with refined occupancies of 0.794 (9) and 0.206 (9).

Related literature

For background literature concerning RuII complexes containing polypyridyl ligands, see: Kalyanasundaram (1982[Kalyanasundaram, K. (1982). Coord. Chem. Rev. 46, 159-244.]); Juris et al. (1988[Juris, A., Balzani, V., Barigelletti, F., Campagna, S., Belser, P. & von Zelewsky, A. (1988). Coord. Chem. Rev. 84, 85-277.]); Concepcion et al. (2008[Concepcion, J. J., Jurss, J. W., Templeton, J. L. & Meyer, T. J. (2008). J. Am. Chem. Soc. 130, 16462-16463.]). For some other RuII complexes containing the 2,2'-bipyridine-4,4'-dicarboxylic acid-N,N' ligand, see: Caspar et al. (2004[Caspar, R., Musatkina, L., Tatosyan, A., Amouri, H., Gruselle, M., Guyard-Duhayon, C., Duval, R. & Cordier, C. (2004). Inorg. Chem. 43, 7986-7993.]); Eskelinen et al. (2000[Eskelinen, E., Luukkanen, S., Haukka, M., Ahlgren, M. & Pakkanen, T. A. (2000). J. Chem. Soc. Dalton Trans. pp. 2745-2752.]); Fujihara et al. (2004[Fujihara, T., Kobayashi, A., Iwai, M. & Nagasawa, A. (2004). Acta Cryst. E60, m1172-m1174.]); Pearson et al. (2008[Pearson, P., Bond, A. M., Deacon, G. B., Forsyth, C. & Spiccia, L. (2008). Inorg. Chim. Acta, 361, 601-612.]); Philippopoulos et al. (2007[Philippopoulos, A. I., Terzis, A., Raptopoulou, C. P., Catalano, V. J. & Falaras, P. (2007). Eur. J. Inorg. Chem. pp. 5633-5644.]). Synthesis details for the precursor RuCl3(terpy) are given in Takeuchi et al. (1984[Takeuchi, K. J., Thompson, M. S., Pipes, D. W. & Meyer, T. J. (1984). Inorg. Chem. 19, 1404-1407.]).

[Scheme 1]

Experimental

Crystal data

  • [RuCl(C15H11N3)(C12H8N2O4)]ClO4·C2H6O·H2O

  • Mr = 777.53

  • Triclinic, [P \overline 1]

  • a = 8.7132 (5) Å

  • b = 11.9207 (7) Å

  • c = 15.9015 (8) Å

  • [alpha] = 90.913 (2)°

  • [beta] = 104.110 (2)°

  • [gamma] = 97.677 (2)°

  • V = 1585.44 (15) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.73 mm-1

  • T = 180 K

  • 0.20 × 0.12 × 0.10 mm
Data collection

  • Bruker-Nonius X8 APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2003[Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.]) Tmin = 0.792, Tmax = 0.931

  • 22443 measured reflections

  • 5961 independent reflections

  • 4978 reflections with I > 2[sigma](I)

  • Rint = 0.031
Refinement

  • R[F2 > 2[sigma](F2)] = 0.040

  • wR(F2) = 0.112

  • S = 1.08

  • 5961 reflections

  • 462 parameters

  • 73 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.91 e Å-3

  • [Delta][rho]min = -0.74 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O2-H2...O1S 0.85 1.75 2.601 (5) 179
O2-H2...O1T 0.85 1.93 2.545 (18) 129
O4-H4...O1Wi 0.85 1.72 2.569 (4) 179
O1W-H1W...O1ii 0.85 1.87 2.720 (4) 179
O1W-H2W...O2Ciii 0.85 1.95 2.795 (12) 178
O1S-H1S...O2Aiv 0.85 2.14 2.986 (8) 180
O1T-H1T...O2Dv 0.85 1.84 2.69 (3) 180
Symmetry codes: (i) -x, -y+1, -z+1; (ii) -x+1, -y+2, -z+1; (iii) x-1, y+1, z; (iv) -x+2, -y+1, -z+1; (v) -x+1, -y+1, -z+1.

Data collection: APEX2 (Bruker-Nonius, 2004)[Bruker-Nonius (2004). APEX2. Bruker-Nonius BV, Delft, The Netherlands.]; cell refinement: SAINT (Bruker, 2003[Bruker (2003). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS5031 ).

Acknowledgements

We are grateful to the Danish Natural Sciences Research Council and the Carlsberg Foundation for provision of the X-ray equipment.

References

Bruker (2003). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker-Nonius (2004). APEX2. Bruker-Nonius BV, Delft, The Netherlands.
Caspar, R., Musatkina, L., Tatosyan, A., Amouri, H., Gruselle, M., Guyard-Duhayon, C., Duval, R. & Cordier, C. (2004). Inorg. Chem. 43, 7986-7993.  [ISI] [CrossRef] [PubMed] [ChemPort]
Concepcion, J. J., Jurss, J. W., Templeton, J. L. & Meyer, T. J. (2008). J. Am. Chem. Soc. 130, 16462-16463.  [PubMed] [ChemPort]
Eskelinen, E., Luukkanen, S., Haukka, M., Ahlgren, M. & Pakkanen, T. A. (2000). J. Chem. Soc. Dalton Trans. pp. 2745-2752.  [CrossRef]
Fujihara, T., Kobayashi, A., Iwai, M. & Nagasawa, A. (2004). Acta Cryst. E60, m1172-m1174.  [CSD] [CrossRef] [details]
Juris, A., Balzani, V., Barigelletti, F., Campagna, S., Belser, P. & von Zelewsky, A. (1988). Coord. Chem. Rev. 84, 85-277.  [CrossRef] [ChemPort] [ISI]
Kalyanasundaram, K. (1982). Coord. Chem. Rev. 46, 159-244.  [CrossRef] [ChemPort] [ISI]
Pearson, P., Bond, A. M., Deacon, G. B., Forsyth, C. & Spiccia, L. (2008). Inorg. Chim. Acta, 361, 601-612.  [CrossRef] [ChemPort]
Philippopoulos, A. I., Terzis, A., Raptopoulou, C. P., Catalano, V. J. & Falaras, P. (2007). Eur. J. Inorg. Chem. pp. 5633-5644.
Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Takeuchi, K. J., Thompson, M. S., Pipes, D. W. & Meyer, T. J. (1984). Inorg. Chem. 19, 1404-1407.

Acta Cryst (2012). E68, m77-m78   [ doi:10.1107/S1600536811054195 ]

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