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Issue 10, 2002
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Synthesis and characterization of perhalogenated diazaphosphametalletidines containing transition metals from group 4 and 5

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Abstract

The preparation and characterization of the novel perhalogenated diazaphosphametalletidines, Cl3M[N(SiMe3)PCl2N(SiMe3)]·THF, M = Ti, Zr and Hf 2–4 and Cl4Nb[N(SiMe3)PCl2N(SiMe3)] 5 are reported. In addition, a new high yield preparation of the previously synthesized metallacycle Cl3Ti[N(SiMe3)PCl2N(SiMe3)] 1 is described. All reported complexes were synthesized by [3 + 1] cyclocondensation reactions involving the aminoiminophosphorane, (Me3Si)2NPCl2[double bond, length as m-dash]NSiMe3, and corresponding metal halides in dichloromethane. When 2.5 equivalents of (Me3Si)2NPCl2[double bond, length as m-dash]NSiMe3 were reacted with NbCl5 a complex series of products was identified by 31P{1H} NMR spectroscopy; crystals of the unusual heterocycles [Cl3Nb{N(SiMe3)PCl2N}2Cl2Nb{N(SiMe3)PCl2N(SiMe3)}] 6 and [Cl2Nb{N(SiMe3)PCl2N(SiMe3)}]2-μ-Cl(NPCl2N) 7 were isolated. Complex 7 contains the first example of a ClNbNPNNb six-membered ring. Structural characterization by single-crystal X-ray diffraction is also reported for metallacycles 2, 3, and 5–7.

Graphical abstract: Synthesis and characterization of perhalogenated diazaphosphametalletidines containing transition metals from group 4 and 5

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Publication details

The article was received on 30 Oct 2001, accepted on 08 Mar 2002 and first published on 19 Apr 2002


Article type: Paper
DOI: 10.1039/B109905C
J. Chem. Soc., Dalton Trans., 2002, 2173-2179

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    Synthesis and characterization of perhalogenated diazaphosphametalletidines containing transition metals from group 4 and 5

    E. Rivard, A. R. McWilliams, A. J. Lough and I. Manners, J. Chem. Soc., Dalton Trans., 2002, 2173
    DOI: 10.1039/B109905C

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