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The niobium oxoazides [NbO(N3)3], [NbO(N3)3·2CH3CN], [(bipy)NbO(N3)3], Cs2[NbO(N3)5] and [PPh4]2[NbO(N3)5]

Research paper by Ralf Haiges, Monica Vasiliu, David A. Dixon, Karl O. Christe

Indexed on: 21 May '16Published on: 11 May '16Published in: Dalton Transactions



Abstract

Niobium oxotriazide, [NbO(N3)3], was prepared in a fluoride–azide exchange reaction between [NbOF3] and an excess of Me3SiN3 in SO2 solution. In acetonitrile solution, the fluoride–azide exchange resulted in the isolation of the adduct [NbO(N3)3·2CH3CN]. The subsequent reaction of [NbO(N3)3] with 2,2′-bipyridine (bipy) resulted in the isolation of the bipyridine adduct [(bipy)NbO(N3)3]. The pentaazido anion [NbO(N3)5]2− was obtained by the reaction of [NbO(N3)3] with two equivalents of ionic azide. The novel niobium oxoazides were fully characterized by their vibrational spectra, impact, friction and thermal sensitivity data and, in the case of [(bipy)NbO(N3)3], Cs2[NbO(N3)5], and [PPh4]2[NbO2(N3)5] by their X-ray crystal structures.

Graphical abstract 10.1039/C6DT01479H.gif