Issue 3, 1990

The chemistry of niobium and tantalum dithiocarbamato-complexes. Part 1. Synthesis, structure, and protonation of dinitrogen-bridged complexes

Abstract

Convenient, ‘single pot’ syntheses of [{MCl3(thf)2}2(µ-N2)](M = Nb or Ta, thf = tetrahydrofuran), using (Me3Si)2NN(SiMe3)2 and Me3SiNHNHSiMe3 respectively, have been achieved. The reaction of these dinitrogen complexes with an excess of SiMe3(S2CNEt2) gives the corresponding [{M(S2CNEt2)3}2(µ-N2)], and the X-ray crystal structure of the complex with M = Nb has been determined. Treatment of the dithiocarbamato-complexes with an excess of anhydrous HX (X = Cl or Br) gives a stoicheiometric yield of hydrazine and the corresponding [M(S2CNEt2)3X2]; the crystal structure of one such example, M = Ta, X = Br, has been determined. Attempts to obtain crystals of [NbCl2(S2CNEt2)3] suitable for X-ray crystallographic analysis resulted in the isolation of [Nb(S2CNEt2)4]2[NbCl5S], whose identity was established crystallographically. Niobium-93 n.m.r. spectroscopy has been used to identify the nature of solution species in the reactions of [{Nb(S2CNEt2)3}2(µ-N2)] with acid.

Article information

Article type
Paper

J. Chem. Soc., Dalton Trans., 1990, 1077-1085

The chemistry of niobium and tantalum dithiocarbamato-complexes. Part 1. Synthesis, structure, and protonation of dinitrogen-bridged complexes

J. R. Dilworth, R. A. Henderson, A. Hills, D. L. Hughes, C. Macdonald, A. N. Stephens and D. R. M. Walton, J. Chem. Soc., Dalton Trans., 1990, 1077 DOI: 10.1039/DT9900001077

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