Macropolyhedral boron-containing cluster chemistry. Assessment of the possibilities of thermolytic mixed-cluster fusion, and of the use of synchrotron X-radiation for the examination of small single crystals of metallaboranes. Isolation and structure of eighteen-vertex [7-(CO)-7,7-(PMe₃)₂-syn-7-IrB₁₇ H₂₀] 

Abstract

Thermolysis of [(CO)(PMe₃)₂HIrB₈H₁₂] with molten B₁₀H₁₄ resulted in small yields of eighteen-vertex [7-(CO)-7,7-(PMe₃)₂-syn-7-IrB₁₇ H₂₀] for which a small crystal was examined by single-crystal diffraction analysis, using synchrotron X-radiation, in order to determine the molecular structure.

References

1. J. Plešek, S. Heřmánek, B. Štíbr and F. Hanousek, Collect. Czech. Chem. Commun., 1967, 32, 1096; J. Plešek, S. Heřmánek and F. Hanousek, Collect. Czech. Chem. Commun., 1968, 33, 699; J. P. Dobson, P. C. Keller and R. Schaefer, Inorg. Chem., 1968, 7, 399.
2. T. Jelínek, J. D. Kennedy and B. Štíbr, J. Chem. Soc., Chem. Commun., 1994, 1415; P. Kaur, J. Holub, N. P. Rath, J. Bould, L. Barton and J. D. Kennedy, Chem. Commun., 1996, 273.
3. M. A. Beckett, J. E. Crook, N. N. Greenwood and J. D. Kennedy, J. Chem. Soc., Dalton Trans., 1986, 1579.
4. M. A. Beckett, N. N. Greenwood, J. D. Kennedy, P. A. Salter and M. Thornton-Pett, J. Chem. Soc., Chem. Commun., 1986, 556.
5. L. Barton, J. Bould, J. D. Kennedy and N. P. Rath, J. Chem. Soc., Dalton Trans., 1996, 3145.
6. J. Bould, unpublished work; J. Bould, N. P. Rath and L. Barton, Organometallics, 1996, 15, 4916.
7. J. Bould, J. E. Crook, N. N. Greenwood and J. D. Kennedy, J. Chem. Soc., Dalton Trans., 1984, 1903.
8. R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, J. V. Flaherty, G. N. Greaves, I. Burrows, D. J. Taylor, S. J. Teat and M. Hamichi, J. Synchrotron Rad., 1997, in the press.
9. G. M. Sheldrick, Acta Crystallogr., Sect. A, 1990, 46, 467.
10. G. M. Sheldrick, SHELXL 93, Program for refinement of crystal structures, University of Göttingen, 1993.
11. H. D. Flack, Acta Crystallogr., Sect. A, 1983, 39, 876.
12. C. K. Johnson, ORTEP, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, TN, 1976; P. McArdle, J. Appl. Crystallogr., 1995, 28, 65.
13. L. G. Sneddon, J. C. Huffman, R. O. Schaeffer and W. Estreib, J. Chem. Soc., Chem. Commun., 1972, 474; E. Mizusawa, S. E. Rudnick and K. Eriks, Inorg. Chem., 1980, 19, 1188.
14. X. L. R. Fontaine, N. N. Greenwood, J. D. Kennedy, P. MacKinnon and M. Thornton-Pett, J. Chem. Soc., Chem. Commun., 1986, 1111; S. O. Kang and L. G. Sneddon, Inorg. Chem., 1988, 27, 587.
15. X. L. R. Fontaine, N. N. Greenwood, J. D. Kennedy, I. Macpherson and M. Thornton-Pett, J. Chem. Soc., Chem. Commun., 1987, 476; P. A. Salter, Ph.D. Thesis, University of Leeds, 1988; P. A. Salter, N. N. Greenwood, J. D. Kennedy and M. Thornton-Pett, unpublished work; U. Doerfler, J. D. Kennedy, L. Barton, C. M. Collins and N. P. Rath, J. Chem. Soc., Dalton Trans., 1997, 707.