Skip to main content
Log in

Reactions of triosmium clusters with indole: X-ray structures of [Os3(CO)10(μ-OH)(μ-OMeCO)] and [Os3(μ-H)(CO)10(μ-1, 2-η2-NC8H6)]

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

Abstract

Treatment of [Os3(CO)12] with indole in presence of a methanolic solution of Me3NO⋅2H2O at 60C afforded the previously reported compounds [(μ-H)Os3(CO)10(μ-OMe)] 2, [(μ-H)Os3(CO)10(μ-OH)] 3 and [Os3(CO)10(μ-OH)(μ-OMeCO)] 4 in 10, 5 and 20% yields, respectively. The reaction of [Os3(CO)10(MeCN)2] with indole at room temperature gave [(μ-H)Os3(CO)10(μ-1,2-η2-NC8H6)] 5 in 40% yield. Compounds 4 and 5 have been characterized by single crystal X-ray diffraction studies. Compound 4 crystallizes in the monoclinic space group P2(1)/c with a = 23.1239(3), b = 9.8087(4), c = 16.9017(6) Å, β = 92.6998(14), Z = 8 and V = 3829.3(2) Å3 and 5 crystallizes in the monoclinic space group P2(1)/c with a = 9.009(3), b = 9.764(4), c = 24.906(6) Å, β = 93.452(14), Z = 4 and V = 2186.9(13) Å3. Compound 4 consists of an open cluster of three osmium atoms with the hydroxy and methoxycarbonyl ligands bridging the open Os–Os edge. Compound 5 consists of an isosceles triangle of osmium atoms with one elongated Os–Os edge which is bridged by the hydride and the indolyl ligands.

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

Access this article

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

Instant access to the full article PDF.

Similar content being viewed by others

References

  1. Eisenstadt, A.; Giandomenico, C.M.; Frederick, M.F.; Laine, R.M. Organometallics 1985, 4, 2033.

    Article  Google Scholar 

  2. Kabir, S.E.; Kolwaite, D.S.; Rosenberg, E.; Hardcastle, K.I.; Cresswell, W.J. Gindstaff, Organometallics 1995, 14, 3611.

    Article  Google Scholar 

  3. Bergman, B.; Holmquist, J.; Smith, R.; Rosenberg, E.; Ciurash, J.; Hardcastle, K.I.; Visi, M. J. Am. Chem. Soc. 1998, 120, 12818.

    Article  Google Scholar 

  4. Abedin, M.J.; Bergman, B.; Holmquist, R.; Smith, R.; Rosenberg, E.; Ciurash, J.; Hardcastle, K.I.; Roe, J.; Vazqez, V.; Roe, V.; Kabir, S.E.; Roy, B.; Alam, S.; Azam, K.A. Coord. Chem. Rev. 1999, 190–192, 975.

  5. Arcia, E.; Kolwaite, D.S.; Rosenberg, E.; Hardcastle, K.I.; Ciurash, J.; Duque, R.; Gobetto, R.; Milone, L.; Osella, D.; Botto, M.; Dastru, W.; Viale, A.; Fiedler, I. Organometallics 1998, 17, 415.

    Article  Google Scholar 

  6. Hardcastle, K.I.; Mianassian, H.; Arce, A.J.; De Sanctis, Y.; Demming, A.J. J. Organomet. Chem. 1989, 386, 119.

    Article  Google Scholar 

  7. Kabir, S.E.; Kolwaite, D.S.; Rosenberg, E.; Scott, L.G.; McPhillips, T.; Duque, R.; Day, M.; Hardcastle, K.I. Organometallics 1996, 15, 1979.

    Article  Google Scholar 

  8. Johnson, B.F.G.; Lewis, J.; Pippard, D.A. J. Chem. Soc. Dalton Trans. 1981, 407.

  9. Hooft, R. COLLECT Data Collection Software; Nonius B.V., Delft: The Netherlands, 1998.

  10. Otwinowski, Z.; Minor, W. In Macromolecular Crystallography; Carter, C.W. Jr.; Sweet, R.M., Eds.; Academic Press: New York, 1997; pp 307–326.

  11. Walker, N.P.C.; Stuart, D. Acta Crystallogr. 1993, A39, 158.

    Google Scholar 

  12. Sheldrick, G.M. Acta Crystallogr. 1990, A46, 467.

    Google Scholar 

  13. Sheldrick, G.M. SHELXL-97 Program for Crystal Structure Refinement; University Göttingen: Germany, 1997.

    Google Scholar 

  14. Agarwala, R.; Azam, K.A.; Dilshad, R.; Kabir, S.E.; Miah, R.; Shahiduzzaman, M.; Hardcastle, K.I.; Rosenberg, E.; Hursthouse, M.B.; Malik, K.M.A. J. Organomet. Chem. 1995, 492, 135.

    Article  Google Scholar 

  15. Johnson, B.F.G.; Lewis, J.; Kilty, O.A. J. Chem. Soc. A 1968, 2869.

  16. (a) Arce, A.J.; Deeming, A.J.; Donovan-Mtunzi, S.; Kabir, S.E. J. Chem. Soc. Dalton Trans. 1985, 2479. (b) Dossi, C.; Fusi, A.; Pizzotti, M.; Psaro, R. Organometallics 1990, 9, 1994.

  17. Knoeppel, D.W.; Chung, J.-H.; Shore, S.G. Acta Crystallogr. 1995, C51, 42.

    Google Scholar 

  18. Churchill, M.R.; Wasserman, H.J. Inorg. Chem. 1980, 19, 2391.

    Article  Google Scholar 

  19. Abedin, S.M.T.; Azam, K.A.; Hursthouse, M.B.; Kabir, S.E.; Malik, K.M.A.; Miah, R.; Vahrenkamp, H. J. Organomet. Chem. 1998, 564, 133.

    Article  Google Scholar 

  20. Jensen, C.M.; Knobler, C.B.; Kaesz, H.D. J. Am. Chem. Soc. 1984, 106, 5926.

    Article  Google Scholar 

  21. Johnson, B.F.G.; Lewis, J.; Raithby, P.R.; Odiaka, T.I. J. Organomet. Chem. 1981, 216, 56.

    Article  Google Scholar 

  22. Hodge, S.R.; Johnson, B.F.G.; Lewis, J.; Raithby, P.R. J. Chem. Soc. Dalton Trans. 1987, 931.

  23. Mingos, D.M.P.; May, A.S. In The Chemistry of Metal Cluster Complexes; Shriver, D.F.; Kaesz, H.D.; Adams, R.D., Eds.; VCH: New York, 1990; pp 11–114.

  24. Churchill, M.R.; DeBoer, B.G. Inorg. Chem. 1977, 16, 878.

    Article  Google Scholar 

  25. Bruce, M.I. In Comprehensive Organometallic Chemistry; Wilkinson, G.; Stone, F.G.A.; Abel, E.W., Eds.; Vol. 5, Pergamon Press, Oxford, 1982; p 4.

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Shariff E. Kabir.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Begum, N., Hyder, M.I., Hossain, G.M.G. et al. Reactions of triosmium clusters with indole: X-ray structures of [Os3(CO)10(μ-OH)(μ-OMeCO)] and [Os3(μ-H)(CO)10(μ-1, 2-η2-NC8H6)]. J Chem Crystallogr 35, 799–807 (2005). https://doi.org/10.1007/s10870-005-4333-7

Download citation

  • Received:

  • Accepted:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10870-005-4333-7

Keywords

Navigation