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DOI: 10.1039/A605378E (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1997, 863-868

Synthesis and reactivity of non-polymeric tetracarboxylatochloro-diruthenium(II,III) complexes. Crystal structure of [Ru2Cl(µ-O2CCHMe2)4 (OPPh3)][hair space]

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M. Carmen Barral, Reyes Jiménez-Aparicio, José L. Priego, Elia C. Royer, Francisco A. Urbanos and Ulises Amador

Abstract

New non-polymeric diruthenium(II,III) carboxylates of the type [Ru2Cl(µ-O2CR)4] (R = CHEt21, CHMeEt 2 or CHMePh 3) were obtained by reaction of HO2CR with [Ru2Cl(µ-O2CMe)4] in methanol–water. The mixed-ligand complex [Ru2Cl(µ-O2CMe)2(µ-O2 CCMe3)2] 4 has also been prepared. The reactivity of these complexes and of the previously described [Ru2Cl(µ-O2CR)4] (R = CMe35 or CHMe26) has been studied and compared with those found for polymeric [Ru2Cl(µ-O2CR)4] (R = alkyl or aryl). The interaction of AgSCN with [Ru2Cl(µ-O2CR)4] or [Ru2Cl(µ-O2CMe)2(µ-O2 CCMe3)2] leads to [Ru2(µ-O2CR)4(SCN)] (R = CHEt27, CHMePh 8 or CMe39) and [Ru2(µ-O2CMe)2(µ-O2 CCMe3)2(SCN)] 10 respectively. The first derivatives of the type [Ru2X(µ-O2CR)4(OPPh3)] (X = Cl; R = CHEt211, CHMeEt 12, CHMePh 13, CMe314 or CHMe215; X = SCN; R = CHEt217, CHMePh 18 or CMe319) and [Ru2Cl(µ-O2CMe)2(µ-O2 CCMe3)2(OPPh3)] 16 containing two different axial ligands have been obtained. Cationic compounds of the type [Ru2(µ-O2CR)4(thf)2]BF 4 (R = CMe320 or CHMe221; thf = tetrahydrofuran), [Ru2(µ-O2CCHMe2)4(OPPh 3)2]BF422 or [Ru2(µ-O2CCHMe2)4(OPPh 3)(thf)]BF423 were also prepared. The crystal structure of 15 has been determined by X-ray crystallography. It has two ruthenium atoms linked by four bridging isobutyrate ligands with the axial positions being occupied by one chlorine atom and one OPPh3 molecule.

References

  1. F. A. Cotton and R. A. Walton, Multiple Bonds Between Metal Atoms, Oxford University Press, Oxford, 2nd edn., 1993 Search PubMed.
  2. M. J. Bennett, K. G. Caulton and F. A. Cotton, Inorg. Chem., 1969, 8, 1 CrossRef CAS.
  3. B. K. Das and A. R. Chakravarty, Polyhedron, 1991, 10, 491 CrossRef CAS.
  4. M. McCann, A. Carvill, P. Guinan, P. Higgings, J. Campbell, H. Ryan, M. Walsh, G. Ferguson and J. Gallagher, Polyhedron, 1991, 10, 2273 CrossRef CAS.
  5. A. Bino, F. A. Cotton and T. R. Felthouse, Inorg. Chem., 1979, 18, 2599 CrossRef CAS.
  6. T. Togano, M. Mukaida and T. Nomura, Bull. Chem. Soc. Jpn., 1980, 53, 2085 CAS.
  7. D. S. Martin, R. A. Newman and L. M. Vlasnik, Inorg. Chem., 1980, 19, 3404 CrossRef CAS.
  8. F. A. Cotton, Y. Kim and T. Ren, Polyhedron, 1993, 12, 607 CrossRef CAS.
  9. M. C. Barral, R. Jiménez-Aparicio, E. C. Royer, C. Ruiz-Valero, M. J. Saucedo and F. A. Urbanos, Inorg. Chem., 1994, 33, 2692 CrossRef CAS.
  10. M. C. Barral, R. Jiménez-Aparicio, J. L. Priego, E. C. Royer, M. J. Saucedo, F. A. Urbanos and U. Amador, J. Chem. Soc., Dalton Trans., 1995, 2183 RSC.
  11. W. J. Geary, Coord. Chem. Rev., 1971, 7, 81 CrossRef CAS.
  12. M. Mukaida, T. Nomura and T. Ishimori, Bull. Chem. Soc. Jpn., 1972, 45, 2143 CAS.
  13. F. A. Urbanos, M. C. Barral and R. Jiménez-Aparicio, Polyhedron, 1988, 7, 2597 CrossRef CAS.
  14. M. C. Barral, R. Jiménez-Aparicio, C. Rial, E. C. Royer, M. J. Saucedo and F. A. Urbanos, Polyhedron, 1990, 9, 1723 CrossRef CAS.
  15. M. C. Barral, R. Jiménez-Aparicio, J. L. Priego, E. C. Royer, E. Gutiérrez-Puebla and C. Ruiz-Valero, Polyhedron, 1992, 11, 2209 CrossRef CAS.
  16. J. Tesler and R. S. Drago, Inorg. Chem., 1984, 23, 3114 CrossRef CAS.
  17. F. A. Cotton, Y. Kim and T. Ren, Polyhedron, 1993, 12, 607 CrossRef CAS.
  18. F. A. Cotton and T. Ren, Inorg. Chem., 1995, 34, 3190 CrossRef CAS.
  19. G. J. Norman, G. E. Renzoni and D. A. Case, J. Am. Chem. Soc., 1979, 101, 5256 CrossRef CAS.
  20. V. M. Miskowsky and H. B. Gray, Inorg. Chem., 1988, 27, 2501 CrossRef CAS.
  21. F. D. Cukiernik, A. Giroud-Godquin, P. Maldivi and J. Marchon, Inorg. Chim. Acta, 1994, 215, 203 CrossRef CAS.
  22. C. K. Johnson, ORTEP, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, TN, 1976.
  23. M. C. Barral, R. Jiménez-Aparicio, E. C. Royer, C. Ruiz-Valero and F. A. Urbanos, Polyhedron, 1989, 8, 2571 CrossRef.
  24. M. C. Barral, R. Jiménez-Aparicio, J. L. Priego, E. C. Royer, M. J. Saucedo and F. A. Urbanos, Polyhedron, 1995, 14, 2419 CrossRef CAS.
  25. R. W. Mitchell, A. Spencer and G. Wilkinson, J. Chem. Soc., Dalton Trans., 1973, 846 RSC.
  26. International Tables for X-Ray Crystallography, Kynoch Press, Birmingham, 1974, vol. 4, pp. 72–98 Search PubMed.
  27. N. Walker and D. Stuart, Acta Crystallogr., Sect. A, 1983, 39, 158 CrossRef.
  28. J. M. Stewart, F. A. Kundell and J. C. Baldwin, The X-RAY 80 System, Computer Science Center, University of Maryland, College Park, MD, 1980.
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