View PDF Version
 
DOI: 10.1039/A606193A (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1997, 509-518

Seven co-ordinate macrocyclic tetrathioether complexes of molybdenum(II) and tungsten(II)

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

Paul K. Baker, Marcus C. Durrant, Sharman D. Harris, David L. Hughes and Raymond L. Richards

Abstract

Treatment of [{Mo(µ-Br)Br(CO)4}2] with 3,3,7,7,11,11,15,15-octamethyl-1,5,9,13-tetrathiacyclohexadecane (Me8[16]aneS4) in CH2Cl2 gave the crystallographically characterised, seven-co-ordinate, ionic complex [MoBr(CO)2(Me8[16]aneS4)][MoBr3 (CO)4] 1. Reaction of 2 equivalents of [MI2(CO)3(NCMe)2] (M = Mo or W) with 1 equivalent of Me8[16]aneS4 afforded the analogous iodo-complex [MoI(CO)2(Me8[16]aneS4)][MoI3 (CO)4] 2 and the crystallographically characterised complexes [WI(CO)2(Me8[16]aneS4)][WI3 (CO)4] 3 and [WI(CO)3(Me8[16]aneS4)][WI3 (CO)4] 4. The cations in complexes 1 and 3 have distorted capped-trigonal-prismatic geometries whereas that in 4 has a geometry lying between capped octahedral and capped trigonal prismatic. The anions of all three complexes have capped-octahedral geometries. Treatment of 2 equivalents of [MI2(CO)3(NCMe)2] with 1 equivalent of 1,5,9,13-tetrathiacyclohexadecane ([16]aneS4), 1,4,8,11-tetrathiacyclotetradecane ([14]aneS4) or 1,4,7,10-tetrathiacyclododecane ([12]aneS4) yielded the bimetallic thioether-bridged complexes [M2I4(CO)6([n]aneS4 -S,S′,S″,S ‴)] (n = 16, M = Mo; n = 14, M = Mo or W; n = 12, M = Mo), and the ionic complexes [WI(CO)2([n]aneS4)][WI3(CO) 4] (n = 16 or 12). The relationships between the various products of these reactions are discussed. Reaction of [16]aneS4 with [MoCl3(thf)3] (thf = tetrahydrofuran) gave a polymeric complex of empirical formula [Mo3Cl9([16]aneS4)2] plus the dinuclear, ionic complex [Mo2Cl5([16]aneS4-S,S ′)2]Cl.

References

  1. T. Yoshida, T. Adachi, M. Kaminaka and T. Ueda, J. Am. Chem. Soc., 1988, 110, 4872 CrossRef CAS.
  2. 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.
  3. D. Sevdić and L. Fekete, Polyhedron, 1985, 4, 1371 CrossRef CAS.
  4. J. J. Chistensen, D. J. Eatough and R. M. Izatt, Chem. Rev., 1974, 74, 351 CrossRef.
  5. S. R. Cooper, Acc. Chem. Res., 1988, 21, 141 CrossRef CAS.
  6. R. E. De Simone, J. Cragel, W. H. Ilsley and M. D. Glick, J. Coord. Chem., 1979, 9, 167 CAS.
  7. J. Cragel, V. B. Pett, M. D. Glick and R. E. De Simone, Inorg. Chem., 1978, 17, 2885 CrossRef CAS.
  8. S. R. Cooper and S. C. Rawle, Struct. Bonding (Berlin), 1990, 72, 1 CAS and refs. therein.
  9. T. Yoshida, T. Adachi, T. Ueda, M. Watanabe, M. Kaminaka and T. Higuchi, Angew. Chem., Int. Ed. Engl., 1987, 26, 1171 CrossRef.
  10. T. Yoshida, T. Adachi and T. Ueda, Pure Appl. Chem., 1990, 62, 1127 CAS.
  11. T. Adachi, N. Sasaki, T. Ueda, M. Kaminaka and T. Yoshida, J. Chem. Soc., Chem. Commun., 1989, 1320 RSC.
  12. T. Yoshida, T. Adachi, T. Ueda, M. Kaminaka, N. Sasaki, T. Higuchi, T. Aoshima, I. Mega, Y. Mizobe and M. Hidai, Angew. Chem., Int. Ed. Engl., 1989, 28, 1040 CrossRef.
  13. A. Hills, D. L. Hughes, M. Jimenez-Tenorio, G. J. Leigh, A. Houlton and J. Silver, J. Chem. Soc., Chem. Commun., 1989, 1774 RSC.
  14. T. E. Jones, L. S. W. L. Sokol, D. B. Rorabacher and M. D. Glick, J. Chem. Soc., Chem. Commun., 1979, 140 RSC.
  15. D. Sevdić, M. Ćurić and Lj. Tušek-Božić, Polyhedron, 1989, 8, 505 CrossRef CAS.
  16. M. C. Durrant, D. L. Hughes, R. L. Richards, P. K. Baker and S. D. Harris, J. Chem. Soc., Dalton Trans., 1992, 3399 RSC.
  17. P. K. Baker, M. C. Durrant, B. Goerdt, S. D. Harris, D. L. Hughes and R. L. Richards, J. Organomet. Chem., 1994, 469, C22 CrossRef.
  18. F. A. Cotton, L. R. Falvello and J. H. Meadows, Inorg. Chem., 1985, 24, 514 CrossRef CAS.
  19. E. O. Fischer, R. Reitmeier, G. Müller and J. Riede, J. Organomet. Chem., 1986, 311, 91 CrossRef CAS.
  20. D. L. Lewis and S. J. Lippard, J. Am. Chem. Soc., 1975, 97, 2697 CrossRef CAS.
  21. M. G. B. Drew and A. P. Wolters, J. Chem. Soc., Chem. Commun., 1972, 457 RSC.
  22. T. Krawinkel and M. C. Durrant, unpublished work.
  23. R. B. King, Inorg. Chem., 1964, 3, 1039 CrossRef CAS.
  24. P. K. Baker, S. J. Coles, M. C. Durrant, S. D. Harris, D. L. Hughes, M. B. Hursthouse and R. L. Richards, J. Chem. Soc., Dalton Trans., 1996, 4003 RSC.
  25. E. Dockal, L. Diaddario, M. D. Glick and D. Rorabacher, J. Am. Chem. Soc., 1977, 99, 4532 CrossRef.
  26. G. J. Grant, J. P. Carpenter, W. N. Setzer and D. G. Van Derveer, Inorg. Chem., 1989, 28, 4128 CrossRef CAS.
  27. P. K. Baker, S. D. Harris, M. C. Durrant, D. L. Hughes and R. L. Richards, J. Chem. Soc., Dalton Trans., 1994, 1401 RSC.
  28. R. Colton and C. J. Rix, Aust. J. Chem., 1969, 22, 305 CAS.
  29. R. Poli and H. D. Mui, J. Am. Chem. Soc., 1990, 112, 2446 CrossRef CAS.
  30. M. C. Durrant, R. L. Richards and S. Firth, J. Chem. Soc., Perkin Trans. 2, 1993, 445 RSC and refs. therein.
  31. C. J. Joung, J. A. Broomhead and C. J. Boreham, J. Organomet. Chem., 1984, 260, 91 CrossRef.
  32. M. C. Durrant, B. Goerdt, C. Hauser, T. Krawinkel and R. L. Richards, Transition Met. Chem., 1995, 20, 583 CrossRef CAS.
  33. A. J. Blake, R. O. Gould, C. Radek and M. Schröder, J. Chem. Soc., Dalton Trans., 1995, 4045 RSC.
  34. J. A. Broomhead, J. Budge and W. Grumbley, Inorg. Synth., 1990, 28, 145 CAS.
  35. P. K. Baker, S. G. Fraser and E. M. Keys, J. Organomet. Chem., 1986, 309, 319 CrossRef CAS.
  36. G. M. Sheldrick, SHELX 76, program for crystal structure determination, University of Cambridge, 1976; extended version, SHELXN, 1977.
  37. G. M. Sheldrick, Acta Crystallogr., Sect. A, 1990, 46, 467 CrossRef.
  38. International Tables for X-Ray Crystallography, Kynoch Press, Birmingham, 1974, vol. 4, pp. 99 and 149 Search PubMed.
  39. S. N. Anderson, R. L. Richards and D. L. Hughes, J. Chem. Soc., Dalton Trans., 1986, 245 RSC.
Click here to see how this site uses Cookies. View our privacy policy here.