View PDF Version
 
DOI: 10.1039/A809853K (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1999, 1077-1084

Synthesis, spectroscopic and structural studies on transition metal carbonyl complexes of cyclic di- and tetra-selenoether ligands

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

Maxwell K. Davies, Marcus C. Durrant, William Levason, Gillian Reid and Raymond L. Richards

Abstract

Reaction of [M(CO)4(nbd)] (M = Cr or Mo, nbd = norbornadiene) or [W(CO)4(TMPA)] (TMPA = N,N,N′,N′-tetramethyl-1,3-propanediamine) with [8]aneSe2 (1,5-diselenacyclooctane) yielded the cis-disubstituted tetracarbonyl species [M(CO)4([8]aneSe2)] (M[hair space][hair space]=[hair space][hair space]Cr, Mo or W). The complexes [M′X(CO)5] (M′[hair space][hair space]=[hair space][hair space]Mn, X[hair space][hair space]=[hair space][hair space]Cl, Br or I; M′[hair space][hair space]=[hair space][hair space]Re, X[hair space][hair space]= Cl or Br) reacted similarly with [8]aneSe2 to give fac-[M′X(CO)3([8]aneSe2)] in high yield. Infrared and multinuclear NMR spectroscopic studies confirmed these assignments and indicated a single species in solution; δ(55Mn) lies in the same range as observed for other fac-[MnX(CO)3(diselenoether)] complexes, while for all of the compounds δ(77Se) is to low frequency of [8]aneSe2 itself (δ 137). Crystal structures of [W(CO)4([8]aneSe2)], [MnBr(CO)3([8]aneSe2)] and [ReBr(CO)3([8]aneSe2)] show the cyclic diselenoether chelating and adopting a chair-boat conformation. The compounds [16]aneSe4 (1,5,9,13-tetraselenacyclohexadecane) and L (1,6-diselena-3,4-benzocyclononane) reacted with the metal(II) species [{MoBr2(CO)4)}2] or [MI2(CO)3(NCMe)2] in CH2Cl2 solution to give seven-co-ordinate [{MoX2(CO)3}2([16]aneSe4)], [WI2(CO)3([16]aneSe4)], [MoX2(CO)3(L)] and [WI2(CO)3(L)], although these species decompose rapidly in co-ordinating solvents. Reaction of [16]aneSe4 with two molar equivalents of [M′Cl(CO)5] yielded the dinuclear complex [{MnCl(CO)3}2([16]aneSe4)] (in which the tetraselenoether is thought to bind in a bidentate manner to each Mn) and the mononuclear complex [ReCl(CO)3([16]aneSe4)] (which is thought to involve bidentate ligation to [16]aneSe4 with two free Se donors). The cationic species fac-[Mn(CO)3(η3-[16]aneSe4)]CF3SO3 was generated by treatment of [MnCl(CO)5] with AgCF3SO3 in Me2CO followed by addition of [16]aneSe4.

References

  1. R. J. Batchelor, F. W. B. Einstein, I. D. Gay, J.-H. Gu, B. D. Johnston and B. M. Pinto, J. Am. Chem. Soc., 1989, 111, 6852 CrossRef.
  2. R. J. Batchelor, F. W. B. Einstein, I. D. Gay, J.-H. Gu, B. M. Pinto and X.-M. Zhou, Inorg. Chem., 1996, 35, 3667 CrossRef CAS.
  3. R. J. Batchelor, F. W. B. Einstein, I. D. Gay, J.-H. Gu, B. M. Pinto and X.-M. Zhou, J. Am. Chem. Soc., 1990, 112, 3706 CrossRef CAS.
  4. R. J. Batchelor, F. W. B. Einstein, I. D. Gay, J.-H. Gu, B. M. Pinto and X.-M. Zhou, J. Organomet. Chem., 1991, 411, 147 CrossRef CAS.
  5. W. Levason, J. J. Quirk and G. Reid, J. Chem. Soc., Dalton Trans., 1996, 3713 RSC; P. F. Kelly, W. Levason, G. Reid and D. J. Williams, J. Chem. Soc., Chem. Commun., 1993, 1716 RSC.
  6. N. R. Champness, P. F. Kelly, W. Levason, G. Reid, A. M. Z. Slawin and D. J. Williams, Inorg. Chem., 1995, 34, 651 CrossRef CAS; C. S. Frampton, W. Levason, J. J. Quirk and G. Reid, Inorg. Chem., 1994, 33, 3120.
  7. N. R. Champness, J. J. Quirk, W. Levason, G. Reid and C. S. Frampton, Polyhedron, 1995, 14, 2753 CrossRef CAS.
  8. W. Levason, G. Reid and S. M. Smith, Polyhedron, 1997, 16, 4253 CrossRef CAS.
  9. W. Levason, J. J. Quirk, G. Reid and S. M. Smith, J. Chem. Soc., Dalton Trans., 1997, 3719 RSC.
  10. D. G. Booth, W. Levason, J. J. Quirk, G. Reid and S. M. Smith, J. Chem. Soc., Dalton Trans., 1997, 3493 RSC.
  11. M. K. Davies, W. Levason and G. Reid, J. Chem. Soc., Dalton Trans., 1998, 2185 RSC.
  12. T. Yoshida, T. Adachi, T. Ueda, M. Watanabe, M. Kaminaka and T. Higuchi, Angew. Chem., Int. Ed. Engl., 1987, 26, 1171 CrossRef; T. Yoshida, T. Adachi, M. Kaminaka and T. Ueda, J. Am. Chem. Soc., 1988, 110, 4872 CrossRef CAS; T. Adachi, N. Sasaki, T. Ueda, M. Kaminaka and T. Yoshida, J. Chem. Soc., Chem. Commun., 1989, 1320 RSC.
  13. T. Adachi, M. C. Durrant, D. L. Hughes, C. J. Pickett, R. L. Richards, J. Talarmin and T. Yoshida, J. Chem. Soc., Chem. Commun., 1992, 1464 RSC.
  14. J. Connolly, M. K. Davies and G. Reid, J. Chem. Soc., Dalton Trans., 1998, 3833 RSC.
  15. P. K. Baker, M. C. Durrant, S. D. Davies, D. L. Hughes and R. L. Richards, J. Chem. Soc., Dalton Trans., 1997, 509 RSC.
  16. B. Rys, H. Duddeck and M. Hiegemann, J. Heterocycl. Chem., 1992, 29, 967 CAS.
  17. B. Rys, H. Duddeck and M. Hiegemann, Tetrahedron, 1991, 47, 1417 CrossRef CAS.
  18. CHEM-X, Chemical Design Ltd., Oxon, July 1996 version.
  19. R. D. Adams and K. T. McBride, Chem. Commun., 1997, 525 RSC; G. W. Bushnell and R. H. Mitchell, Can. J. Chem., 1982, 60, 362 CAS; T. Okajima, Z. H. Wang and Y. Fukazawa, Tetrahedron Lett., 1989, 30, 1551 CrossRef CAS; M. Iwaoka, H. Komatsu and S. Tomoda, Bull. Chem. Soc. Jpn., 1996, 69, 1825 CAS.
  20. K. Ohno, H. Matsuura and H. Murata, J. Mol. Struct., 1980, 66, 45 CrossRef CAS; J. R. Alkins and P. J. Hendra, Spectrochim. Acta, 1966, 22, 2075 CrossRef.
  21. W. C. Still and I. Galynker, Tetrahedron, 1981, 37, 3981 CrossRef CAS; Y. Fukazawa, S. Usui and Y. Uchio, Tetrahedron Lett., 1986, 27, 1825 CrossRef CAS.
  22. P. K. Baker, A. I. Clark, M. M. Meehan, E. E. Parker, A. E. Underhill, M. G. B. Drew, M. C. Durrant and R. L. Richards, Transition Met. Chem., 1998, 23, 155 CrossRef CAS.
  23. P. K. Baker, S. D. Harris, M. C. Durrant, D. L. Hughes and R. L. Richards, J. Chem. Soc., Dalton Trans., 1994, 1401 RSC.
  24. R. Uson, V. Riera, J. Gimeno, M. Laguna and M. P. Gamasa, J. Chem. Soc., Dalton Trans., 1979, 996 RSC.
  25. J. Connolly, W. Levason, S. D. Orchard, S. J. A. Pope and G. Reid, unpublished work.
  26. J. Connolly, G. W. Goodban, G. Reid and A. M. Z. Slawin, J. Chem. Soc., Dalton Trans., 1998, 2225 RSC; W. Levason, S. D. Orchard and G. Reid, Organometallics, in the press Search PubMed.
  27. E. W. Abel, S. K. Bhargava, M. M. Bhatti, K. Kite, M. A. Mazid, K. G. Orrell, V. Sik, B. L. Williams, M. B. Hursthouse and K. M. A. Malik, J. Chem. Soc., Dalton Trans., 1982, 2065 RSC.
  28. F. A. Cotton, D. J. Darensbourg, S. Klein and B. W. S. Kilthammer, Inorg. Chem., 1982, 21, 2661 CrossRef CAS.
  29. K. J. Reimer and A. Shaver, Inorg. Synth., 1979, 19, 159.
  30. S. P. Schmidt, W. C. Trogler and F. Basolo, Inorg. Synth., 1990, 28, 160 CAS.
  31. J. J. Eisch and R. B. King, Organomet. Synth., 1965, 1, 123 Search PubMed.
  32. G. R. Dobson and G. C. Faber, Inorg. Chim. Acta, 1987, 4, 87 CrossRef CAS.
  33. J. A. Broomhead, J. Budge and W. Grumley, Inorg. Synth., 1990, 28, 145 CAS.
  34. P. K. Baker, S. G. Fraser and E. M. Keys, J. Organomet. Chem., 1986, 309, 319 CrossRef CAS.
  35. H. Werner and R. Prinz, Chem. Ber., 1967, 100, 265 CAS.
  36. PATTY, The DIRDIF Program System, P. T. Beurskens, G. Admiraal, G. Beurskens, W. P. Bosman, S. Garcia-Granda, R. O. Gould, J. M. M. Smits and C. Smykalla, Technical Report of the Crystallography Laboratory, University of Nijmegen, 1992.
  37. TEXSAN, Crystal Structure Analysis Package, Molecular Structure Corporation, Houston, TX, 1995.
  38. H. D. Flack, Acta Crystallogr., Sect. A, 1983, 39, 876 CrossRef.
Click here to see how this site uses Cookies. View our privacy policy here.