Synthesis of Some d0 Organoimido Complexes of the Early Transition Metals

Inorganic Chemistry

Volumn 22, Issue 6, 1983, Pages 965-969

  Nugent, William A ^a  

^a DUPONT COMPANY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0000118641     PISSN: 00201669     EISSN: 1520510X     Source Type: Journal    
DOI: 10.1021/ic00148a023     Document Type: Article

References (23)

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7. Rappe, A.K.; Goddard, W. A. J. Am. Chem. Soc. 1982, 104, 448-456.
8. (a) Nugent, W.A.; Harlow, R. L. J. Chem. Soc., Chem. Commun. 1978, 579-580. (b) Nugent, W. A.; Harlow, R. L. J. Chem. Soc., Chem. Commun. 1979, 342-343. (c) Nugent, W. A.; Harlow, R. L. J. Chem. Soc., Chem. Commun. 1979, 1105-1106. (d) Nugent, W. A.; Harlow, R. L. Inorg. Chem. 1979, 18, 2030-2032. (e) Nugent, W. A.; Harlow, R. L. Inorg. Chem. 1980, 19, 777-779. (f) Nugent, W. A.; Harlow, R. L.; McKinney, R. J. J. Am. Chem. Soc. 1979, 101, 7265-7268.
9. Nugent, W.A.; Haymore, B. L. Coord. Chem. Rev. 1980, 31, 123-175.
10. For Group. 5 imido complexes: (a) Wiberg, N.; Haring, H.-W.; Schubert, U. Z. Naturforsch., B: Anorg. Chem., Org. Chem. 1980, 35B, 599-603. (b) Churchill, M. R.; Wasserman, H. J. Inorg. Chem. 1982, 21, 223-226. (c) Lemenovskii, D. A.; Konde, S. A.; Perevalova, E. G. J. Organomet. Chem. 1982, 226, 223-227. (d) Preuss, F.; Towae, W. Z. Naturforsch., B: Anorg. Chem., Org. Chem. 1981, 36B, 1130-1135.
11. For group. 6 imido complexes: (a) Dehmcke, K.; Weiher, U.; Fenske, D. Z. Anorg. Allg. Chem. 1979, 456, 71-80. (b) Anorg. Allg. Chem. 1979, 457, 105-114. (c) Weller, F.; Muller, U.; Weiher, U.; Dehnicke, K. Anorg. Allg. Chem. 1980, 460, 191-199. (d) Korswagen, R.; Weidenhammer, K.; Ziegler, M. I. Z. Naturforsch., B. Anorg. Chem., Org. Chem. 1979, 34B, 1507-1511. (e) Korswagen, R.; Ziegler, M. I. Anorg. Chem., Org. Chem. 1980, 35B, 1196-1200. (f) Henderson, R. A.; Davies, G.; Dilworth, J. R. J. Chem. Soc, Dalton Trans. 1981, 40-50. (g) Chisholm, M. H.; Folting, K.; Huffmann, J. C.; Kirkpatrick, C. C.; Ratermann, A. L. Inorg. Chem. 1982, 21, 978-982. (h) Edelblut, A. W.; Wentworth, R. A. D. Inorg. Chem. 1980, 19, 2006-2010. (i) Inorg. Chem. 1980, 19, 1100-1117. (j) Maata, E. A.; Haymore, B. L.; Wentworth, R. A. D. Inorg. Chem. 1980, 19, 1055-1059. (k) Sevan, P. C.; Chatt, J.; Dilworth, J. R.; Henderson, R. A.; Leigh, G. J. J. Chem. Soc, Dalton Trans. 1982, 821-824.
12. For group. 7 imido complexes: (a) Weiher, U.; Dehnicke, K.; Fenske, D. Z. Anorg. Allg. Chem. 1979, 457, 115-122. (b) La Monica, G.; Cenini, S. J. Chem. Soc, Dalton Trans. 1980, 1145-1149. (c) La Monica, G.; Cenini, S.; Porta, F. Inorg. Chim. Acta 1981, 48, 91-95. (d) Chiu, K. W.; Wong, W.-K.; Wilkinson, G.; Galas, A. M. R.; Hursthouse, M. B. Polyhedron 1982, 1, 37-44.
13. Bradley, D.C.; Chisholm, M. H. Acc. Chem. Res. 1976, 9, 273-280.
14. Chatt, J.; Choukroun, R.; Dilworth, J. R.; Hyde, J.; Vella, P.; Zubieta, J. Transition Met. Chem. (Weinheim, Ger.) 1979, 4, 59-63.
15. Schmidt, M.; Schmidbauer, H. Angew. Chem. 1959, 71, 220.
16. Pike, R.M. J. Org. Chem. 1961, 26, 232-236.
17. (a) A rearrangement similar to that in eq 4 has been demonstrated for a phosphorus(V) (trimethylsilyl)amide: Neilson, R. H.; Jacobs, R. D.; Scheirman, R. W.; Wilburn, J. C. Inorg. Chem. 1978, 17, 1880-1882. (b) This synthetic approach is based on the work of Bürger and coworkers. They reported IR and NMR evidence that the reaction of NaN(SiMe3)2 with VOCl3 afforded [(Me3Si)2N]2(Me3SiO)V-(NSiMe3): Burger, H.; Smrekar, O.; Wannagat, U. Monatsh. Chem. 1964, 95, 292-302.
18. A monomeric model for this structure gave an R index of approximately 0.06, but the complex appears disordered. Unit cell parameters at-47 °C are a = 12.840 (5) A, b = 9.362 (3) A, and c = 18.333 (6) A, and the probable space group is orthorhombic, Pbcn.
19. The compound is unfortunately disordered, and a model of the predicted structure would refine only to an R index of approximately 0.12. The determination was further complicated by an apparent second phase, which was present independent of the method used to grow the crystals. Weissenberg photographs gave a second set of diffuse spots that could not be indexed on the basis of the standard unit cell. At-98 °C the parameters found are as follows: a - 21.000 (4) A, i = 7.602 (2) A, c = 14.852 (3) A, ß “106.89 (1)°, monoclinic, space group C2.
20. Schmidt, M.; Schmidbauer, H. Inorg. Synth. 1967, 9, 149-151.
21. Kauer, J. C. U.S. Patent 3 546290.
22. Nugent, W.A.; McKinney, R. J.; Kasowski, R. V.; Van-Catledge, F. A. Inorg. Chim. Acta Lett. 1982, 65, L91-L93.
23. Schmidt, M.; Schmidbauer, H. Angew. Chem. 1958, 70, 704. Abel, E. W. Z. Naturforsch., B: Anorg. Chem., Org. Chem., Biochem., Biophys., Biol. 1960, 15B, 57.