Molecular dynamics of (η6-arene)tricarbonylchromium complexes in the solid state: carbon-13 nuclear magnetic resonance and crystal structure of [Cr(η6-C6HMe5)(CO)3]

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Patrick J. Barrie, Christiana A. Mitsopoulou, Majid Motevalli and Edward W. Randall


Abstract

Variable-temperature solid-state 13C NMR spectra have been recorded for a series of [Cr(η6-arene)(CO)3] complexes. In all cases there is evidence for carbonyl exchange in the solid state at elevated temperatures. Both the isotropic chemical shifts and the chemical shift anisotropies of the 13CO groups were obtained. The relative ease of the carbonyl exchange depended on the extent of methyl substitution of the arene ring. It was more facile in those complexes with less symmetric arene rings. The single-crystal structure of [Cr(η6-C6HMe5)(CO)3] was determined at 150 K. X-Ray data recorded at room temperature led to a misleading structural refinement due to molecular motion.


References

  1. D. Braga and F. Grepioni, Chem. Commun., 1996, 571 RSC.
  2. D. Braga, Chem. Rev., 1992, 92, 633 CrossRef CAS.
  3. M. J. McGlinchey, Adv. Organomet. Chem., 1992, 34, 285 CAS.
  4. C. A. Fyfe, Solid State NMR for Chemists, C.F.C. Press, Guelph, 1983 Search PubMed.
  5. P. J. Barrie, C. A. Mitsopoulou and E. W. Randall, J. Chem. Soc., Dalton Trans., 1995, 2125 RSC.
  6. A. D. Hunter and J. L. McLernon, Organometallics, 1989, 8, 2679 CrossRef CAS.
  7. J. F. Haw, G. C. Campbell and R. C. Crosby, Anal. Chem., 1986, 58, 3172 CrossRef CAS.
  8. J. Herzfeld and A. E. Berger, J. Chem. Phys., 1980, 73, 6021 CrossRef CAS.
  9. G. E. Hawkes, K. D. Sales, L. Y. Lian and R. Gobetto, Proc. R. Soc. London, Ser. A, 1989, 424, 93 CAS.
  10. U. Haeberlen, Adv. Magn. Reson. Suppl., 1976, 1, 9 Search PubMed.
  11. G. M. Sheldrick, SHELXS 86, University of Göttingen, 1986.
  12. G. M. Sheldrick, SHELXL 93, University of Göttingen, 1993.
  13. A. C. North, D. C. Phillips and F. S. Mathews, Acta Crystallogr., Sect. A, 1968, 24, 351 CrossRef.
  14. A. L. Spek, PLUTON, University of Utrecht, 1990.
  15. G. E. Hawkes, K. D. Sales, S. Aime, R. Gobetto and L. Y. Lian, Inorg. Chem., 1991, 30, 1489 CrossRef CAS.
  16. G. W. Wagner and B. E. Hanson, Inorg. Chem., 1987, 26, 2019 CrossRef CAS.
  17. M. Mehring, High Resolution NMR Spectroscopy in Solids, Springer, Berlin, 1983 Search PubMed.
  18. H. J. Buttery, G. Keeling, S. F. A. Kettle, I. Paul and P. J. Stamper, J. Chem. Soc. A, 1969, 2224 RSC.
  19. C. K. Johnson, ORTEP, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, TN, 1976.
  20. M. F. Bailey and L. F. Dahl, Inorg. Chem., 1965, 4, 1298 CrossRef CAS.
  21. M. F. Bailey and L. F. Dahl, Inorg. Chem., 1965, 4, 1314 CrossRef CAS; B. Rees and P. Coppens, Acta Crystallogr., Sect. B, 1931, 29, 2515 Search PubMed; Y. Wang, K. Angermund, R. Goddard and C. Krüger, J. Am. Chem. Soc., 1987, 109, 587 CrossRef CAS.
  22. F. van Meurs and H. van Koningsveld, J. Organomet. Chem., 1977, 131, 423 CrossRef CAS.
  23. A. E. Aliev, K. D. M. Harris, F. Guillaume and P. J. Barrie, J. Chem. Soc., Dalton Trans., 1994, 3193 RSC.
  24. D. F. Brougham, P. J. Barrie, G. E. Hawkes, I. Abrahams, M. Motevalli, D. A. Brown and G. J. Long, Inorg. Chem., 1996, 35, 5595 CrossRef CAS.
  25. D. Braga and F. Grepioni, J. Chem. Soc., Dalton Trans., 1990, 3143 RSC.
  26. D. Braga and F. Grepioni, Polyhedron, 1990, 9, 53 CrossRef CAS.
  27. S. Aime, D. Braga, R. Gobetto, F. Grepioni and A. Orlandi, Inorg. Chem., 1991, 30, 951 CrossRef CAS.
  28. D. E. Koshland, S. E. Meyers and J. P. Chesik, Acta Crystallogr., Sect. B, 1977, 33, 2013 CrossRef.
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