Skip to main content
SpringerLink
Log in

Bridging and chelating diphosphine ligands in Ru3(μ-H)(μ-N=CPh2)(CO)8(P—P). X-ray diffraction structures of Ru3(μ-H)(μ-N=CPh2)(CO)8(dmpe) and Ru3(μ-H)(μ-N=CPh2)(CO)8(bpcd)

  • Published:
Journal of Chemical Crystallography Aims and scope Submit manuscript

Abstract

Treatment of the azavinylidene-bridged cluster Ru3(μ-H)(μ-N=CPh2)(CO)10 (1) with the diphosphine ligand bis(dimethylphosphino)ethane (dmpe) gives Ru3( μ-H)(μ-N=CPh2)(CO)8(dmpe) (2) in moderate yield, while the ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) reacts with Ru3( μ-H)(μ-N=CPh2)(CO)10 in the presence of Me3NO to furnish Ru3( μ-H)(μ-N=CPh2)(CO)8(bpcd) (3) in low yield. Each new cluster has been isolated and characterized in solution by IR and NMR (1H and 31P) spectroscopies, and the coordination mode exhibited by the ancillary diphosphine ligand in 2 and 3 has been established by X-ray crystallography. Ru3( μ-H)(μ-N=CPh2)(CO)8(dmpe) crystallizes in the monoclinic space group P2(1)/c, a = 10.791(1) Å, b = 16.377(1) Å, c = 18.148(1) Å, β = 96.675(2)°, V = 3185.3(4) Å3, Z = 4, D cacl = 1.791 Mg/m3; R = 0.0360, R w = 0.0866 for 7522 observed reflections with I > 2σ(I). Ru3(μ-H)(μ-N=CPh2)(CO)8(bpcd) crystallizes, as the CH2Cl2 solvate, in the triclinic space group \(P\bar 1\), a = 11.956(1) Å, b = 14.228(1) Å, c = 31.409(3) Å, α = 89.377(2)°, β = 79.344(2)°, γ = 77.235(2)°, V = 5118.4(8) Å3, Z = 2, D calc = 1.670 Mg/m3; R = 0.0557, R w = 0.1069 for 10977 observed reflections with I > 2σ(I). The structural details of clusters 2 and 3 are contrasted with Ru3(μ-H)(μ-N=CPh2)(CO)7(μ-dppm)(η-dppm), which is the only known structurally characterized phosphine-substituted cluster of this genre.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. Andreu, P.L.; Cabeza, J.A.; del Río, I.; Riera, B.C. Organometallics 1996, 15, 3004.

    Google Scholar 

  2. Cabeza, J.A.; del Río, I.; Riera, V. J. Organomet. Chem. 1997, 548, 255.

    Google Scholar 

  3. Bois, C.; Cabeza, J.A.; Franco, R.J.; Riera, V.; Saborit, E. J. Organomet. Chem. 1998, 564, 201.

    Google Scholar 

  4. Cabeza, J.A.; del Río, I.; Franco, R.J.; Grepioni, F.; Riera, V. Organometallics 1997, 16, 2763.

    Google Scholar 

  5. Cabeza, J.A.; del Río, I.; Moreno, M.; Riera, V. Organometallics 1998, 17, 3027.

    Google Scholar 

  6. Schulman, C.L.; Richmond, M.G.; Watson, W.H.; Nagl, A. J. Organomet. Chem. 1989, 368, 367.

    Google Scholar 

  7. Don, M.-J.; Richmond, M.G.; Watson, W.H.; Krawiec, M.; Kashyap, R.P. J. Organomet. Chem. 1991, 418, 231.

    Google Scholar 

  8. Shen, H.; Bott, S.G.; Richmond, M.G. Organometallics 1995, 14, 4625.

    Google Scholar 

  9. Bott, S.G.; Shen, H.; Richmond, M.G. Struct. Chem. 2001, 12, 225.

    Google Scholar 

  10. Shen, H.; Williams, T.J.; Bott, S.G.; Richmond, M.G. J. Organomet. Chem. 1995, 505, 1.

    Google Scholar 

  11. Bruce, M.I.; Jensen, C.M.; Jones, N.L. Inorg. Synth. 1989, 26, 259.

    Google Scholar 

  12. Kofron, W.G.; Baclawski, L.M. Org. Chem. 1976, 41, 1879.

    Google Scholar 

  13. Fenske, D.; Becher, H.J. Chem. Ber. 1975, 108, 2115.

    Google Scholar 

  14. Roedig, A.; Hörnig, L. Chem. Ber. 1955, 88, 2003.

    Google Scholar 

  15. Shriver, D.F. The Manipulation of Air-Sensitive Compounds; McGraw-Hill: New York, 1969.

    Google Scholar 

  16. Saint, version 6.02; Bruker Analytical X-ray Systems, Inc. Copyright 1997–1999.

  17. SHELXTL, version 5.1; Bruker Analytical X-ray Systems, Inc. Copyright 1998.

  18. Speck, A.L. PLATON–A Multipurpose Crystallographic Tool; Utrecht University: Utrecht, The Netherlands, 2001.

    Google Scholar 

  19. Kolle, U. J. Organomet. Chem. 1977, 133, 53.

    Google Scholar 

  20. Albers, M.O.; Coville, N.J. Coord, Chem. Rev. 1984, 53, 227.

    Google Scholar 

  21. Shen, H.; Bott, S.G.; Richmond, M.G. J. Chem. Crystallogr. 1997, 27, 25.

    Google Scholar 

  22. Shen, H.; Williams, T.J.; Bott, S.G.; Richmond, M.G. J. Organomet. Chem. 1995, 505, 1.

    Google Scholar 

  23. Gaeda, P.E.; Johnson, B.F.G.; McPartlin, M.; Pearsall, M.-A. J. Chem. Soc., Dalton Trans. 1996, 4621.

  24. Orpen, A.G.; Brammer, L.; Allen, F.H.; Kennard, O.; Watson, D.G.; Taylor, R. J. Chem. Soc., Dalton Trans. 1989, S1.

  25. Dierkes, P.; van Leeuwen, P.W.N.M. J. Chem. Soc., Dalton Trans. 1999, 1519.

Download references

Author information

Authors and Affiliations

  1. Department of Chemistry, Texas Christian University, Fort Worth, Texas

    William H. Watson & Miguel A. Mendez-Rojas

  2. Department of Chemistry, University of North Texas, Denton, Texas, 76203

    Yuxin Zhao & Michael G. Richmond

Authors
  1. William H. Watson
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Miguel A. Mendez-Rojas
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Yuxin Zhao
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Michael G. Richmond
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Michael G. Richmond.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Watson, W.H., Mendez-Rojas, M.A., Zhao, Y. et al. Bridging and chelating diphosphine ligands in Ru3(μ-H)(μ-N=CPh2)(CO)8(P—P). X-ray diffraction structures of Ru3(μ-H)(μ-N=CPh2)(CO)8(dmpe) and Ru3(μ-H)(μ-N=CPh2)(CO)8(bpcd). Journal of Chemical Crystallography 33, 765–774 (2003). https://doi.org/10.1023/A:1026107407465

Download citation

  • Issue Date:

  • DOI: https://doi.org/10.1023/A:1026107407465

Search

Navigation