Metal (Li, K, SnII and HgII) complexes of the 1,3-diazaallyl [N(R)C(Ph)NC(Ph)[double bond, length half m-dash]CR2] (R = SiMe3)

(Note: The full text of this document is currently only available in the PDF Version )

Peter B. Hitchcock, Michael F. Lappert and Marcus Layh


Abstract

The new lithium 1,3-diazaallyl [Li{N(R)C(Ph)NC(Ph)[double bond, length half m-dash]CR2}] 1 [abbreviated as Li(L–L′)] has been prepared from [Li(CR3)(thf[hair space])2] and 2 equivalents of benzonitrile (R = SiMe3, thf = C4H8O). Compound 1 was shown to be a suitable precursor for the synthesis of the metal complexes [SnCl(L–L′)] 2, [[upper bond 1 start]Sn(L–L[upper bond 1 end]′)2] 3 and [Hg(L–L′)2] 4 from the appropriate metal(II) chloride, while the reduction of 2 with potassium–graphite led in high yield to [{[upper bond 1 start]K(µ-L–L[upper bond 1 end]′)}2] 5. Each of the compounds was fully characterised by multinuclear NMR spectroscopy, mass spectrometry and for 3–5 by X-ray diffraction.


References

  1. M. F. Lappert and D.-S. Liu, J. Organomet. Chem., 1995, 500, 203 CrossRef CAS.
  2. Z. H. Aiube and C. Eaborn, J. Organomet. Chem., 1984, 269, 217 CrossRef CAS.
  3. P. B. Hitchcock, M. F. Lappert and M. Layh, Inorg. Chim. Acta, 1998, 269, 181 CrossRef CAS.
  4. P. B. Hitchcock, J. Hu, M. F. Lappert, M. Layh and J. Severn, Chem. Commun., 1997, 1189 RSC.
  5. P. B. Hitchcock, J. Hu, M. F. Lappert, M. Layh, D.-S. Liu, J. R. Severn and S. Tian, An. Quím., Int. Ed. Engl., 1996, 92, 186 Search PubMed; P. B. Hitchcock, M. F. Lappert and M. Layh, J. Chem. Soc., Dalton Trans., 1998, 1619 RSC.
  6. F. T. Edelmann, Coord. Chem. Rev., 1994, 137, 403 CrossRef.
  7. W. Rüdorff and K. Brodersen, Z. Anorg. Allg. Chem., 1953, 274, 323 CrossRef CAS.
  8. B. Kamenar and D. Grdenić, Inorg. Chim. Acta, 1969, 3, 25 CrossRef CAS.
  9. D. Grdenić, B. Kamenar, M. Sikirica, T. Duplančić, S. Govedić, A. Hergold and P. Matković, Acta Crystallogr., Sect. A, 1975, 31, S132.
  10. A. Zinn, K. Dehnicke, D. Fenske and G. Baum, Z. Anorg. Allg. Chem., 1991, 596, 47 CrossRef CAS.
  11. C. Ergezinger, F. Weller and K. Dehnicke, Z. Naturforsch., Teil B, 1988, 43, 1119 CAS.
  12. W. Hiller, J. Strähle, A. Zinn and K. Dehnicke, Z. Naturforsch., Teil B, 1989, 44, 999 CAS.
  13. (a) C. Ergezinger, F. Weller and K. Dehnicke, Z. Naturforsch., Teil B, 1988, 43, 1621 CAS; (b) R. Duchateau, A. Meetsma and J. H. Teuben, Chem. Commun., 1996, 223 RSC.
  14. J.-K. Buijink, M. Noltemeyer and F. T. Edelmann, Z. Naturforsch., Teil B, 1991, 46, 1328 CAS; D. Stalke, M. Wedler and F. T. Edelmann, J. Organomet. Chem., 1992, 431, C1 CrossRef CAS.
  15. M. Westerhausen and H.-D. Hausen, Z. Anorg. Allg. Chem., 1992, 615, 27 CrossRef CAS.
  16. H. H. Karsch, P. A. Schlüter and M. Reisky, Eur. J. Inorg. Chem., 1998, 433 CrossRef CAS.
  17. T. Fjeldberg, H. Hope, M. F. Lappert, P. P. Power and A. J. Thorne, J. Chem. Soc., Chem. Commun., 1983, 639 RSC.
  18. B. S. Jolly, M. F. Lappert, L. M. Engelhardt, A. H. White and C. L. Raston, J. Chem. Soc., Dalton Trans., 1993, 2653 RSC.
  19. (a) K. F. Tesh, T. P. Hanusa and J. C. Huffman, Inorg. Chem., 1990, 29, 1584 CrossRef CAS; (b) P. G. Williard, Acta Crystallogr., Sect. C, 1988, 44, 270 CrossRef.
  20. P. C. Andrews, D. R. Baker, R. E. Mulvey, W. Clegg and P. A. O'Neil, Polyhedron, 1991, 10, 1839 CrossRef CAS.
  21. A. Steiner and D. Stalke, Inorg. Chem., 1993, 32, 1977 CrossRef CAS.
  22. F. Pauer and D. Stalke, J. Organomet. Chem., 1991, 418, 127 CrossRef CAS.
  23. P. B. Hitchcock, M. F. Lappert and D.-S. Liu, J. Organomet. Chem., 1995, 488, 241 CrossRef CAS.
  24. C. S. Barrett, Acta Crystallogr., 1956, 9, 671 CrossRef CAS.
  25. S. Maier, W. Hiller, J. Strähle, C. Ergezinger and K. Dehnicke, Z. Naturforsch., Teil B, 1988, 43, 1628 CAS.
  26. D. Fenske, G. Baum, A. Zinn and K. Dehnicke, Z. Naturforsch., Teil B, 1991, 45, 1273.
  27. G. M. Sheldrick, SHELXS 86, Program for the Solution of Crystal Structures, University of Göttingen, 1986.
  28. G. M. Sheldrick, SHELXL 93, Program for Crystal Structure Refinement, University of Göttingen, 1993.
Click here to see how this site uses Cookies. View our privacy policy here.