Formation of Mo(NAr)(PMe₃)₂Cl₃and Mo₂(PMe₃)₄Cl₄from Reduction of Mo(NAr)₂Cl₂(DME) with Mg in the Presence of PMe₃[Ar=2,6-diisopropylphenyl]

  • Published : 1997.02.20

Abstract

Magnesium reduction of Mo(N-C6H3-2,6-i-Pr2)2Cl2(DME) in the presence of trimethylphosphine led to a mixture of Mo(N-C6H3-2,6-i-Pr2)(PMe3)2Cl3, 1, and Mo2(PMe3)4Cl4, 2. In solution 1 is slowly air-oxidized to Mo(N-2,6-i-Pr2-C6H3)(OPMe3)(PMe3)Cl3, 3. 1 is chemically inert to carbon nucleophiles (ZnMe2, ZnEt2, AlMe3, AlEt3, LiCp, NaCp, TlCp, NaCp*, MeMgBr, EtMgBr), oxygen nucleophiles (LiOEt, LiO-i-Pr, LiOPh, LiOSPh), and hydrides (LiBEt3H, LiBEt3D). Crystal data for 1: orthorhombic space group P212121, a=11.312(3) Å, b=11.908(3) Å, c=19.381(6) Å, Z=4, R(wR2)=0.0463 (0.1067). Crystal data for 2: monoclinic space group Cc, a=18.384(3) Å, b=9.181(2) Å, c=19.118(3) Å, b=124.98(1)°, Z=4, R(wR2)=0.0228 (0.0568). Crystal data for 3: orthorhombic space group P212121, a=11.464(1) Å, b=14.081(2) Å, c=16.614(3) Å, Z=4, R(wR2)=0.0394 (0.0923).

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References

  1. Prog. Inorg. Chem. v.42 Wigley, D. E.
  2. Coord. Chem. Rev. v.123 Lin, Z.;Hall, M. B.
  3. Inorg. Chem. v.34 Morrison, D. L.;Wigley, D. E.
  4. Inorg. Chem. v.32 Saravanamuthu, A.;Ho, D. M.;Kerr, M. E.;Fitzgerald, C.;Bruce, M. R. M.;Bruce, A. E.
  5. J. Chem. Soc., Dalton Trans. Bradley, D. C.;Hodge, S. R.;Runnacles, J. D.;Hughes, M.;Mason, J.;Richards, R. L.
  6. Polyhedron v.7 Sloan, O. D.;Thornton, P.
  7. J. Am. Chem. Soc. v.101 Nugent, W. A.;Harlow, R. L.;McKinney, R. J.
  8. J. Am. Chem. Soc. v.101 Haymore, B. L.;Maatta, E. A.;Wentworth, R. A. D.
  9. Acta Crystallogr. v.A46 Sheldrick, G. M.
  10. SHELXL-93 Sheldrick, G. M.
  11. J. Am. Chem. Soc. v.103 Cotton, F. A.;Extine, M. W.;Felthouse, T. R.;Kolthammer, B. W. S.;Lay, D. G.
  12. Acc. Chem. Res. v.24 Schrock, R. R.
  13. J. Chem. Soc., Chem. Commun. Bell, A.;Clegg, W.;Dyer, P. W.;Elsegood, M. R. J.;Gibson, V. C.;Marshall, E. L.
  14. J. Chem. Soc., Dalton Trans. Orpen, A. G.;Brammer, L.;Allen, F. H.;Kennard, O.;Watson, D. G.;Taylor, R.
  15. Inorg. Chem. v.29 Minelli, M.;Carson, M. R.;Whisenhunt, D. W.;Imhof, W.;Huttner, G.
  16. The Organometallic Chemistry of the Transition Metals(2nd ed.) Crabtree, R. H.
  17. Organometallics v.10 Bazan, G. C.;Schrock, R. R.;O'Regen, M. B.
  18. Inorg. Chem. v.22 Goeden, G. V.;Haymore, B. L.
  19. J. Am. Chem. Soc. v.114 Cundari, T. R.
  20. J. Organomet. Chem. v.485 Massey, S. T.;Mansour, B.;McElwee-White, L.
  21. Comprehensive Coordination Chemistry v.2 Chisholm, M. H.;Rothwell, I. P.;Wilkinson, G.(ed.);Gillard, R. D.(ed.);McCleverty, J. A.(ed.)
  22. J. Am. Chem. Soc. v.113 Glueck, D. S.;Wu, J.;Hollander, F. J.;Bergman, R. G.
  23. Metal-Ligand Multiple Bonds Nugent, W. A.;Mayer, J. M.
  24. Coord. Chem. Rev. v.31 Nugent, W. A.;Haymore, B. L.
  25. Inorg. Chim. Acta v.8 Cenini, S.;La Monica, G.
  26. J. Am. Chem. Soc. v.31 Fox, H. H.;Yap, K. B.;Robbins, J.;Cai, S.;Schrock, R. R.
  27. J. Am. Chem. Soc. v.113 Arndtsen, B. A.;Sleiman, H. F.;Chang, A. K.;McElwee-White, L.