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Volume 69 
Part 12 
Pages m659-m660  
December 2013  

Received 16 September 2013
Accepted 25 October 2013
Online 13 November 2013

Key indicators
Single-crystal X-ray study
T = 180 K
Mean [sigma](C-C) = 0.005 Å
R = 0.043
wR = 0.089
Data-to-parameter ratio = 17.3
Details
Open access

Chlorido([eta]6-N2-diphenylphosphanyl-N1,N1-diisopropyl-4-methoxybenz­amidine-[kappa]P)(triphenylphosphane-[kappa]P)ruthenium(II) trifluoromethansulfonate acetone disolvate

aLaboratoire de Chimie de Coordination, UPR-CNRS 8241, 205, route de Narbonne, 31077 Toulouse cedex, France
Correspondence e-mail: laure.vendier@lcc-toulouse.fr

In the title compound, [RuCl(C18H15P)(C26H31N2OP)](CF3O3S)·2C3H6O, the RuII ion is coordinated in a three-legged piano stool, half-sandwich-type geometry by a chlorido ligand, a tri­phenyl­phosphine and a tethered [eta]6-(phenyl-p-O-meth­oxy) [kappa]1-P N-di­phenyl­phosphino N'-diisopropyl amidine ligand charge-balanced by a trifluormethansulfonate counter-anion. The [eta]6-coordination mode of the arene incorporated into the structure was generated in situ after addition of methyl tri­fluoro­methane­sulfonate to the neutral [eta]5-arene tethered precursor complex [RuCl(PPh3)([eta]5:[kappa]1-OC6H4C(NiPr2)=N-PPh2)] in di­chloro­methane solution.

Related literature

For related tethered [eta]6-arene ruthenium(II) half-sandwich piano-stool complexes, see: Therrien & Ward (1999[Therrien, B. & Ward, T. R. (1999). Angew. Chem. Int. Ed. 38, 405-408.]); Faller & D'Alliessi (2003[Faller, J. W. & D'Alliessi, D. G. (2003). Organometallics, 22, 2749-2757.]); Cetinkaya et al. (2003[Cetinkaya, B., Demir, S., Ozdemir, I., Toupet, L., Sémeril, D., Bruneau, C. & Dixneuf, P. H. (2003). Chem. Eur. J. 9, 2323-2330.]); Cadierno et al. (2004[Cadierno, V., Díez, J., García-Álvarez, J. & Gimeno, J. (2004). Chem. Commun. pp. 1820-1821.]); Ito et al. (2008[Ito, M., Endo, Y. & Ikariya, T. (2008). Organometallics, 27, 6053-6055.]); Arquier et al. (2009[Arquier, D., Vendier, L., Miqueu, K., Sotiropoulos, J.-M., Bastin, S. & Igau, A. (2009). Organometallics 28, 4945-4957.]); Parekh et al. (2012[Parekh, V., Ramsden, J. A. & Wills, M. (2012). Catal Sci. Technol. 2, 406-414.]). For [eta]5-arene ruthenium(II) half-sandwich piano-stool complexes, see: Cole-Hamilton et al. (1976[Cole-Hamilton, D. J., Young, R. J. & Wilkinson, G. (1976). J. Chem. Soc. Dalton Trans. pp. 1995-2001.]); Rosete et al. (1979[Rosete, R. O., Cole-Hamilton, D. J. & Wilkinson, G. (1979). J. Chem. Soc. Dalton Trans. pp. 1618-1637.]); Snelgrove et al. (2005[Snelgrove, J. L., Conrad, J. C., Eelman, M. D., Moriarty, M. M., Yap, G. P. A. & Fogg, D. E. (2005). Organometallics 24, 103-109.]); Ferrando-Miguel et al. (2005[Ferrando-Miguel, G., Wu, P., Huffman, J. C. & Caulton, K. G. (2005). New J. Chem. 29, 193-204.]). For the increasing medicinal inter­est in [eta]6-arene ruth­enium(II) half-sandwich complexes, see: Hartinger & Dyson (2009[Hartinger, C. G. & Dyson, P. J. (2009). Chem. Soc. Rev. 38, 391-401.]); Allardyce et al. (2001[Allardyce, C. S., Dyson, P. J., Ellis, D. J. & Heath, S. L. (2001). Chem. Commun. pp.1396-1397.]); Scolaro et al. (2005[Scolaro, C., Bergamo, A., Brescacin, L., Delfino, R., Cocchietto, M., Laurenczy, G., Geldbach, T. J., Sava, G. & Dyson, P. J. (2005). J. Med. Chem. 48, 4161-4171.]); Dyson (2007[Dyson, P. J. (2007). Chimia, 61, 698-703.]); Chatterjee et al. (2008[Chatterjee, S., Kundu, S., Bhattacharyya, A., Hartinger, C. G. & Dyson, P. J. (2008). J. Biol. Inorg. Chem. 13, 1149-1155.]). For the synthesis of the precursor, see: Kechaou et al. (2013[Kechaou, M., Vendier, L., Bastin, S., Sotiropoulos, J.-M., Miqueu, K., Menéndez-Rodríguez, L., Crochet, P., Cadierno, V. & Igau, A. (2013). Chem. Commun. Submitted.]).

[Scheme 1]

Experimental

Crystal data
  • [RuCl(C18H15P)(C26H31N2OP)](CF3O3S)·2C3H6O

  • Mr = 1082.51

  • Monoclinic, P 21 /c

  • a = 11.6970 (2) Å

  • b = 15.0260 (3) Å

  • c = 29.7770 (6) Å

  • [beta] = 99.864 (2)°

  • V = 5156.21 (17) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.52 mm-1

  • T = 180 K

  • 0.19 × 0.1 × 0.03 mm

Data collection
  • Oxford Diffraction Xcalibur (Eos, Gemini ultra) diffractometer

  • Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2010[Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]) Tmin = 0.933, Tmax = 0.982

  • 43527 measured reflections

  • 10532 independent reflections

  • 8192 reflections with I > 2[sigma](I)

  • Rint = 0.046

Refinement
  • R[F2 > 2[sigma](F2)] = 0.043

  • wR(F2) = 0.089

  • S = 1.09

  • 10532 reflections

  • 608 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.49 e Å-3

  • [Delta][rho]min = -0.37 e Å-3

Data collection: CrysAlis CCD (Oxford Diffraction, 2010[Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2010[Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]); program(s) used to solve structure: SIR92 (Altomare et al., 1994[Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.]); 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: WinGX publication routines (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CQ2007 ).


Acknowledgements

We thank the French Ministry of Education for a PhD Fellowship for M-KP and the CNRS for financial support. Johnson Matthey is gratefully acknowledged for the loan of RuCl3·xH2O.

References

Allardyce, C. S., Dyson, P. J., Ellis, D. J. & Heath, S. L. (2001). Chem. Commun. pp.1396-1397.  [CSD] [CrossRef]
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.  [CrossRef] [IUCr Journals]
Arquier, D., Vendier, L., Miqueu, K., Sotiropoulos, J.-M., Bastin, S. & Igau, A. (2009). Organometallics 28, 4945-4957.  [CSD] [CrossRef] [ChemPort]
Cadierno, V., Díez, J., García-Álvarez, J. & Gimeno, J. (2004). Chem. Commun. pp. 1820-1821.  [CSD] [CrossRef]
Cetinkaya, B., Demir, S., Ozdemir, I., Toupet, L., Sémeril, D., Bruneau, C. & Dixneuf, P. H. (2003). Chem. Eur. J. 9, 2323-2330.  [PubMed] [ChemPort]
Chatterjee, S., Kundu, S., Bhattacharyya, A., Hartinger, C. G. & Dyson, P. J. (2008). J. Biol. Inorg. Chem. 13, 1149-1155.  [Web of Science] [CrossRef] [PubMed] [ChemPort]
Cole-Hamilton, D. J., Young, R. J. & Wilkinson, G. (1976). J. Chem. Soc. Dalton Trans. pp. 1995-2001.
Dyson, P. J. (2007). Chimia, 61, 698-703.  [CrossRef] [ChemPort]
Faller, J. W. & D'Alliessi, D. G. (2003). Organometallics, 22, 2749-2757.  [CSD] [CrossRef] [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Ferrando-Miguel, G., Wu, P., Huffman, J. C. & Caulton, K. G. (2005). New J. Chem. 29, 193-204.  [ChemPort]
Hartinger, C. G. & Dyson, P. J. (2009). Chem. Soc. Rev. 38, 391-401.  [Web of Science] [CrossRef] [PubMed] [ChemPort]
Ito, M., Endo, Y. & Ikariya, T. (2008). Organometallics, 27, 6053-6055.  [CSD] [CrossRef] [ChemPort]
Kechaou, M., Vendier, L., Bastin, S., Sotiropoulos, J.-M., Miqueu, K., Menéndez-Rodríguez, L., Crochet, P., Cadierno, V. & Igau, A. (2013). Chem. Commun. Submitted.
Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.
Parekh, V., Ramsden, J. A. & Wills, M. (2012). Catal Sci. Technol. 2, 406-414.  [CrossRef] [ChemPort]
Rosete, R. O., Cole-Hamilton, D. J. & Wilkinson, G. (1979). J. Chem. Soc. Dalton Trans. pp. 1618-1637.  [CrossRef]
Scolaro, C., Bergamo, A., Brescacin, L., Delfino, R., Cocchietto, M., Laurenczy, G., Geldbach, T. J., Sava, G. & Dyson, P. J. (2005). J. Med. Chem. 48, 4161-4171.  [Web of Science] [CrossRef] [PubMed] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Snelgrove, J. L., Conrad, J. C., Eelman, M. D., Moriarty, M. M., Yap, G. P. A. & Fogg, D. E. (2005). Organometallics 24, 103-109.  [CSD] [CrossRef] [ChemPort]
Therrien, B. & Ward, T. R. (1999). Angew. Chem. Int. Ed. 38, 405-408.  [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m659-m660   [ doi:10.1107/S1600536813029450 ]

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