Skip to main content
SpringerLink
Log in

Characterization of [Re2Cl3(μ-dppm)2(NCCH3)2][Cl] and [Re2Cl3(μ-dppm)2(NCC6H5)2][Cl]·2CH2Cl2 by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques

  • Published:
Journal of Cluster Science Aims and scope Submit manuscript

Abstract

The complex Re2Cl6(P-n-Bu3)2 prepared in situ reacts with CH3CN to form a blue-green solution. Addition of the chelating phosphine bis(diphenylphosphino)methane (dppm) results in the formation of the complex [Re2Cl3(μ-dppm)2(NCCH3)2][Cl] (1) upon heating. The two acetonitrile molecules adopt a trans geometry on the rhenium center with the axially coordinated chlorine. The analogous trans benzonitrile species [Re2Cl3(μ-dppm)2(NCC6H5)2][Cl]·2CH2Cl2 (2) is synthesized under the same reaction conditions. The coupling constants of the AA′BB′ 31P{1H} NMR spectra of the compounds were elucidated from 31P–31P homonuclear J-resolved NMR experiments. Additional characterization methods include 31P{1H} NMR spectroscopy, UV-vis spectroscopy, and X-ray crystallography.

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. F. A. Cotton, N. F. Curtis, B. F. G. Johnson, and W. R. Robinson (1965). Inorg. Chem. 4, 326.

    Google Scholar 

  2. F. A. Cotton, N. F. Curtis, C. B. Harris, B. F. G. Johnson, S. J. Lippard, J. T. Mague, W. R. Robinson, and J. S. Wood (1964). Science 145, 1305.

    Google Scholar 

  3. F. A. Cotton and R. A. Walton, Multiple Bonds between Metal Atoms (Oxford University Press, 1993). Second Edition.

  4. T. E. Concolino and J. L. Eglin (1997). J. Cluster Sci. 8, 461.

    Google Scholar 

  5. T. E. Concolino, J. L. Eglin, and R. J. Staples (1999). Polyhedron 915.

  6. C. B. Bauer, T. E. Concolino, J. L. Eglin, R. D. Rogers, and R. J. Staples (1998). J. Chem. Soc., Dalton Trans. 2813.

  7. J. L. Eglin, E. M. Hines, E. J. Valente, and J. D. Zubkowski (1995). Inorg. Chim. Acta 229, 113.

    Google Scholar 

  8. G. N. Holder, T. A. Leach, C. T. Eagle, and L. A. Bottomley (1995). Transition Met. Chem. 20, 409.

    Google Scholar 

  9. P. E. Fanwick, J.-S. Qi, K.-Y. Shih, and R. A. Walton (1990). Inorg. Chim. Acta 172, 65.

    Google Scholar 

  10. T. J. Barder, F. A. Cotton, L. R. Falvello, and R. A. Walton (1985). Inorg. Chem. 24, 1258.

    Google Scholar 

  11. D. R. Derringer, K.-Y. Shih, P. E. Fanwick, and R. A. Walton (1991). Polyhedron 10, 79.

    Google Scholar 

  12. D. A. Kort, W. Wu, P. E. Fanwick, and R. A. Walton (1995). Transition Met. Chem. 20, 625.

    Google Scholar 

  13. P. E. Fanwick, A. C. Price, and R. A. Walton (1988). Inorg. Chem. 27, 2601.

    Google Scholar 

  14. P. E. Fanwick, J. Qi, and R. A. Walton (1990). Inorg. Chem. 29, 3787.

    Google Scholar 

  15. W. Wu, P. E. Fanwick, and R. A. Walton (1996). Inorg. Chem. 35, 5484.

    Google Scholar 

  16. K.-Y. Shih, P. E. Fanwick, and R. A. Walton (1993). Organometallics 12, 347.

    Google Scholar 

  17. W. Wu, P. E. Fanwick, and R. A. Walton (1996). J. Cluster Science 7, 155.

    Google Scholar 

  18. W. Wu, P. E. Fanwick, and R. A. Walton (1996). Inorg. Chim. Acta 242, 81.

    Google Scholar 

  19. W. Wu, J. A. Subramony, P. E. Fanwick, and R. A. Walton (1996). Inorg. Chem. 35, 6784.

    Google Scholar 

  20. L. B. Anderson, S. M. Tetrick, and R. A. Walton (1986). J. Chem. Soc., Dalton Trans. 55.

  21. F. A. Cotton, K. R. Dunbar, L. R. Falvello, and R. A. Walton (1985). Inorg. Chem. 24, 4180.

    Google Scholar 

  22. L. B. Anderson, T. J. Barder, F. A. Cotton, K. R. Dunbar, L. R. Falvello, and R. A. Walton (1986). Inorg. Chem. 25, 3629.

    Google Scholar 

  23. L. B. Anderson, T. J. Barder, D. Esjornson, R. A. Walton, and B. E. Bursten (1986). J. Chem. Soc., Dalton Trans. 2607.

  24. D. A. Kort, K.-Y. Shih, W. Wu, P. E. Fanwick, and R. A. Walton (1995). Organometallics 14, 448.

    Google Scholar 

  25. W. Wu, P. E. Fanwick, and R. A. Walton (1995). Inorg. Chem. 34, 5810.

    Google Scholar 

  26. D. Esjornson, D. R. Derringer, P. E. Fanwick, and R. A. Walton (1989). Inorg. Chem. 28, 2821.

    Google Scholar 

  27. T. J. Barder and R. A. Walton (1982). Inorg. Chem. 21, 2510.

    Google Scholar 

  28. International Tables for X-Ray Crystallography (D. Reidel Publishing, 1985).

  29. G. M. Sheldrick (1990). Acta Cryst. A46, 467.

    Google Scholar 

  30. G. M. Sheldrick, Crystallographic Computing (Oxford University Press, 1992).

  31. SMART V 4.043 Software for the CCD Detector System, Siemens Analytical Instruments Division, Madison, WI 1996.

  32. SAINT V 4.035 Software for the CCD Detector System, Siemens Analytical Instruments Division, Madison, WI 1995.

  33. SADABS. Program for Absorption corrections using Siemens CCD based on the method of Bob Blessing. Acta Cryst. A51, 33 (1995).

    Google Scholar 

  34. Sheldrick, G. M. Shelxs-90, Program for the Solution of Crystal Structures, University of Gottingen, Germany, 1986.

    Google Scholar 

  35. Sheldrick, G. M. SHELXL-93, Program for the Refinement of Crystal Structures, University of Gottingen, Germany, 1993.

    Google Scholar 

  36. SHELXTL 5.03 (PC-Version), Program library for Structure Solution and Molecular Graphics, Siemens Analytical Instruments Division, Madison, WI 1995.

  37. R. A. Walton (1989). Polyhedron 8, 1689.

    Google Scholar 

  38. D. Esjornson, P. E. Fanwick, and R. A. Walton (1988). Inorg. Chem. 27, 3066.

    Google Scholar 

  39. W. P. Aue, E. Bartholdi, and R. R. Ernst (1976). J. Chem. Phys. 65, 4226.

    Google Scholar 

  40. J. V. Z. Krevor, U. Simonis, and A. Karson (1992). Inorg. Chem. 31, 312.

    Google Scholar 

  41. G. Wu and R. E. Wasylishen (1996). Inorg. Chem. 35, 3113.

    Google Scholar 

  42. A. G. Sykes and K. R. Mann (1990). Inorg. Chem. 29, 4449.

    Google Scholar 

  43. F. A. Cotton, L. M. Daniels, K. R. Dunbar, L. R. Falvello, S. M. Tetrick, and R. A. Walton (1985). J. Am. Chem. Soc. 107, 3524.

    Google Scholar 

  44. F. A. Cotton, J. L. Eglin, and S.-J. Kang (1993). Inorg. Chem. 32, 2332.

    Google Scholar 

  45. F. A. Cotton, L. R. Falvello, C. A. James, and R. L. Luck (1990). Inorg. Chem. 29, 4759.

    Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Department of Chemistry, Mississippi State University, Mississippi State, Mississippi, 39762

    Thomas E. Concolino, Judith L. Eglin, Chad E. Hadden & Rickey P. Hicks

  2. Department of Chemistry, Harvard University, Cambridge, Massachusetts, 02138

    Richard J. Staples

  3. Department of Chemistry, Mississippi College, Clinton, Mississippi, 39058

    Edward J. Valente

  4. Department of Chemistry, Jackson State University, Jackson, Mississippi, 39217

    Jeffrey D. Zubkowski

Authors
  1. Thomas E. Concolino
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Judith L. Eglin
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Chad E. Hadden
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Rickey P. Hicks
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Richard J. Staples
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Edward J. Valente
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Jeffrey D. Zubkowski
    View author publications

    You can also search for this author in PubMed Google Scholar

Rights and permissions

Reprints and permissions

About this article

Cite this article

Concolino, T.E., Eglin, J.L., Hadden, C.E. et al. Characterization of [Re2Cl3(μ-dppm)2(NCCH3)2][Cl] and [Re2Cl3(μ-dppm)2(NCC6H5)2][Cl]·2CH2Cl2 by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques. Journal of Cluster Science 11, 109–123 (2000). https://doi.org/10.1023/A:1009012731250

Download citation

  • Issue Date:

  • DOI: https://doi.org/10.1023/A:1009012731250

Search

Navigation