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Volume 64 
Part 2 
Pages m309-m310  
February 2008  

Received 12 December 2007
Accepted 3 January 2008
Online 9 January 2008

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Key indicators
Single-crystal X-ray study
T = 120 K
Mean [sigma](C-C) = 0.007 Å
R = 0.049
wR = 0.115
Data-to-parameter ratio = 19.5
Details
Open access

[mu]-Pyrazine-2,5-dicarboxylato-bis[chlorido([eta]6-p-cymene)ruthenium(II)] tert-butanol disolvate

Noelia M. Sanchez Ballester,a Mark R. J. Elsegooda* and Martin B. Smitha

aChemistry Department, Loughborough University, Loughborough, Leicestershire LE11 3TU, England
Correspondence e-mail: m.r.j.elsegood@lboro.ac.uk

A new tert-butanol solvate of [{(iPrC6H4Me)RuCl}2{[mu]-2,5-pyz(COO)2}] (pyz = pyrazine) has been crystallized and structurally characterized. The solvate, [Ru2(C10H14)2(C6H2N2O4)Cl2]·2C4H10O, contains one half-molecule of the ruthenium(II) complex and one molecule of tert-butanol in the asymmetric unit. The complex molecule lies on an inversion centre with the two chlorides trans. In contrast, the previously reported structure was solvent-free. Similar metric parameters are found between the butanol solvate and the solvent-free form and an intermolecular O-H...O hydrogen bond exists between [mu]-pyrazine-2,5-dicarboxylato-bis[chlorido([eta]6-p-cymene)ruthenium(II)] and the tert-butanol molecule.

Related literature

The structure of the solvent-free complex has been reported previously (Govindaswamy et al., 2007[Govindaswamy, P., Therrien, B., Süss-Fink, G., Stepnicka, P. & Ludvík, J. (2007). J. Organomet. Chem. 692, 1661-1671.]). One molecule adopts a trans configuration of the two chloro ligands while the second lies on a twofold axis giving the two chloro ligands a cis configuration. For other related literature, see: Cadierno et al. (2002[Cadierno, V., Díez, J., García-Garrido, S. E., García-Granda, S. & Gimeno, J. (2002). J. Chem. Soc. Dalton Trans. pp. 1465-1472.]); Carter et al. (1993[Carter, L., Davies, D. L., Fawcett, J. & Russell, D. R. (1993). Polyhedron, 12, 1599-1602.]); Dann et al. (2006[Dann, S. E., Durran, S. E., Elsegood, M. R. J., Smith, M. B., Staniland, P. M., Talib, S. & Dale, S. H. (2006). J. Organomet. Chem. 691, 4829-4842.]); Dorcier et al. (2005[Dorcier, A., Dyson, P. J., Gossens, C., Rothlisberger, U., Scopelliti, R. & Tavernelli, I. (2005). Organometallics, 24, 2114-2123.]); Drommi et al. (1995[Drommi, D., Arena, C. G., Nicolò, F., Bruno, G. & Faraone, F. (1995). J. Organomet. Chem. 485, 115-121.]); Ganter (2003[Ganter, C. (2003). Chem. Soc. Rev. 32, 130-138.]); Gemel et al. (2000[Gemel, C., John, R., Slugovc, C., Mereiter, K., Schmid, R. & Kirchner, K. (2000). J. Chem. Soc. Dalton Trans. pp. 2607-2612.]); Grote et al. (2004[Grote, Z., Scopelliti, R. & Severin, K. (2004). J. Am. Chem. Soc. 126, 16959-16972.]); Ion et al. (2006[Ion, L., Morales, D., Pérez, J., Riera, L., Riera, V., Kowenicki, R. A. & McPartlin, M. (2006). Chem. Commun. pp. 91-93.]); Konar et al. (2004[Konar, S., Manna, S. C., Zangrando, E. & Chaudhuri, N. R. (2004). Inorg. Chim. Acta, 357, 1593-1597.]); Lahuerta et al. (1988[Lahuerta, P., Latorre, J., Sanaú, M., Cotton, F. A. & Schwotzer, W. (1988). Polyhedron, 7, 1311-1316.]); Ma et al. (2004[Ma, C., Han, Y. & Zhang, R. (2004). J. Organomet. Chem. 689, 1675-1683.]); Pinto et al. (2004[Pinto, P., Marconi, G., Heinemann, F. W. & Zenneck, U. (2004). Organometallics, 23, 374-380.]).

[Scheme 1]

Experimental

Crystal data

  • [Ru2(C10H14)2(C6H2N2O4)Cl2]·2C4H10O

  • Mr = 855.80

  • Monoclinic, P 21 /c

  • a = 9.8483 (2) Å

  • b = 11.3968 (3) Å

  • c = 16.3448 (3) Å

  • [beta] = 91.465 (2)°

  • V = 1833.93 (7) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 1.01 mm-1

  • T = 120 (2) K

  • 0.18 × 0.04 × 0.03 mm
Data collection

  • Bruker-Nonius Kappa APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2007[Sheldrick, G. M. (2007). SADABS. Version 2007/2. University of Göttingen, Germany.]) Tmin = 0.839, Tmax = 0.970

  • 18492 measured reflections

  • 4195 independent reflections

  • 3594 reflections with I > 2[sigma](I)

  • Rint = 0.046
Refinement

  • R[F2 > 2[sigma](F2)] = 0.049

  • wR(F2) = 0.115

  • S = 1.06

  • 4196 reflections

  • 215 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 2.78 e Å-3

  • [Delta][rho]min = -1.04 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O3-H3...O1 0.84 1.98 2.804 (5) 168

Data collection: COLLECT (Hooft, 1998[Hooft, R. W. W. (1998). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: DENZO (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001[Sheldrick, G. M. (2001). SHELXTL. Version 6.10. Bruker AXS Inc., Madison, Wisconsin, USA.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BV2088 ).

Acknowledgements

The authors acknowledge the Loughborough University Development Fund for the provision of a studentship (to NMSB). The authors are also grateful to the EPSRC National Crystallography Service at the University of Southampton for the data collection.

References

Cadierno, V., Díez, J., García-Garrido, S. E., García-Granda, S. & Gimeno, J. (2002). J. Chem. Soc. Dalton Trans. pp. 1465-1472.  [CrossRef]
Carter, L., Davies, D. L., Fawcett, J. & Russell, D. R. (1993). Polyhedron, 12, 1599-1602.  [CrossRef] [ChemPort]
Dann, S. E., Durran, S. E., Elsegood, M. R. J., Smith, M. B., Staniland, P. M., Talib, S. & Dale, S. H. (2006). J. Organomet. Chem. 691, 4829-4842.  [CrossRef] [ChemPort]
Dorcier, A., Dyson, P. J., Gossens, C., Rothlisberger, U., Scopelliti, R. & Tavernelli, I. (2005). Organometallics, 24, 2114-2123.  [CrossRef] [ChemPort]
Drommi, D., Arena, C. G., Nicolò, F., Bruno, G. & Faraone, F. (1995). J. Organomet. Chem. 485, 115-121.  [CrossRef] [ChemPort]
Ganter, C. (2003). Chem. Soc. Rev. 32, 130-138.  [CrossRef] [PubMed] [ChemPort]
Gemel, C., John, R., Slugovc, C., Mereiter, K., Schmid, R. & Kirchner, K. (2000). J. Chem. Soc. Dalton Trans. pp. 2607-2612.  [CrossRef]
Govindaswamy, P., Therrien, B., Süss-Fink, G., Stepnicka, P. & Ludvík, J. (2007). J. Organomet. Chem. 692, 1661-1671.  [CrossRef] [ChemPort]
Grote, Z., Scopelliti, R. & Severin, K. (2004). J. Am. Chem. Soc. 126, 16959-16972.  [CrossRef] [PubMed] [ChemPort]
Hooft, R. W. W. (1998). COLLECT. Nonius BV, Delft, The Netherlands.
Ion, L., Morales, D., Pérez, J., Riera, L., Riera, V., Kowenicki, R. A. & McPartlin, M. (2006). Chem. Commun. pp. 91-93.  [CrossRef]
Konar, S., Manna, S. C., Zangrando, E. & Chaudhuri, N. R. (2004). Inorg. Chim. Acta, 357, 1593-1597.  [ISI] [CSD] [CrossRef] [ChemPort]
Lahuerta, P., Latorre, J., Sanaú, M., Cotton, F. A. & Schwotzer, W. (1988). Polyhedron, 7, 1311-1316.  [ChemPort]
Ma, C., Han, Y. & Zhang, R. (2004). J. Organomet. Chem. 689, 1675-1683.  [CrossRef] [ChemPort]
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Pinto, P., Marconi, G., Heinemann, F. W. & Zenneck, U. (2004). Organometallics, 23, 374-380.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2001). SHELXTL. Version 6.10. Bruker AXS Inc., Madison, Wisconsin, USA.
Sheldrick, G. M. (2007). SADABS. Version 2007/2. University of Göttingen, Germany.

Acta Cryst (2008). E64, m309-m310   [ doi:10.1107/S1600536808000202 ]

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