Issue 6, 2007

Reactions of manganese and rhenium complexes with organic azides: preparation of tetraazabutadiene derivatives

Abstract

Azide complexes [M(RN3)(CO)3P2]BPh41–3 [M = Mn, Re; R = C6H5CH2, 4-CH3C6H4CH2, C6H5, 4-CH3C6H4, C5H9; P = PPh(OEt)2, PPh2(OEt)] were prepared by allowing tricarbonyl MH(CO)3P2 hydride complexes to react first with Brønsted acid (HBF4, CF3SO3H) and then with organic azide in the dark. In sunlight the reaction yielded tetraazabutadiene [M(η2-1,4-R2N4)(CO)2P2]BPh44–6 complexes or, with benzyl azide, imine [M{η1-NH[double bond, length as m-dash]C(H)Ar}(CO)3P2]BPh47 (Ar = C6H5, 4-CH3C6H4) derivatives. Tetraazabutadiene [M(η2-1,4-R2N4)(CO)2P2]BPh4 complexes were also prepared by reacting dicarbonyl MH(CO)2P3 species first with Brønsted acid and then with an excess of organic azide. Complexes were characterised spectroscopically (IR, 1H, 31P, 13C, 15N NMR data) and by the X-ray crystal structure determination of complex [Re{η2-1,4-(C6H5CH2)2N4}(CO)2{PPh(OEt)2}2]BPh4 (5a). Strong evidence for coordination of the organic azide was obtained from the 15N NMR spectra of labelled [M(C6H5CH215NN15N)(CO)3P2]BPh4 derivatives.

Graphical abstract: Reactions of manganese and rhenium complexes with organic azides: preparation of tetraazabutadiene derivatives

Supplementary files

Article information

Article type
Paper
Submitted
26 Sep 2006
Accepted
11 Dec 2006
First published
09 Jan 2007

Dalton Trans., 2007, 661-668

Reactions of manganese and rhenium complexes with organic azides: preparation of tetraazabutadiene derivatives

G. Albertin, S. Antoniutti, A. Bacchi, A. Celebrin, G. Pelizzi and G. Zanardo, Dalton Trans., 2007, 661 DOI: 10.1039/B613964G

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