Preparation and Spectroscopic Characterisation of a Series of Heterobimetallic N-phenyldiethanolaminate-alkoxide Derivatives of Oxovanadium(V)

Abstract

Reaction of VO(OPri)3 with two equivalents of N-phenyldiethanolamine (PhDEAH2) yields a homometallic complex [VO(PhDEA)(PhDEAH)] 1, which reacts with a number of metal alkoxides to afford heterobimetallic oxovanadium(V) complexes of the types [VO(PhDEA)2{M(OR)n-1}] [where PhDEA = C6H5N(CH2CH2O–)2], [M =: Al (n = 3, R = Pri) 2; Al (n = 3, R = But) 3; Ti (n = 4, R = Pri) 4; Zr (n = 4, R = Pri) 5; Nb (n = 5, R = Pri) 6; Ta (n = 5, R = Pri) 7. The derivative [VO(PhDEA)(OSiPh3)] 8 has been prepared by the equimolar interaction of [VO(PhDEA)(OPri)] with Ph3SiOH. All of these complexes have been characterised by spectroscopic (IR; 1H, 13C, 27Al and 51V NMR) studies, elemental analyses, and molecular weight measurements. The derivative 2 has also been characterised by FAB mass spectral studies, which supports for its monomeric nature.

Synthesis and Spectroscopic Characterisation of a New Class of Heterobimetallic Homoleptic Diethanolaminate Complexes of Niobium(V) and Tantalum(V)

“…9,10 Recently, we have developed a novel route for the synthesis of heterobimetallic alkoxide coordination complexes 11 utilising the higher reactivity of the hydroxy functionality in homometallic complexes derived from polyols such as glycols, di-and triethanolamines. 11 This strategy has been successful in the synthesis of novel heterobimetallic glycolate-, 12,16 diethanolaminate- [17][18][19][20] and triethanolaminate- 13,21,22 isopropoxide complexes. Due to the presence of isopropoxy groups, these types of complexes show a strong propensity for hydrolysis 3,11 even in the presence of only traces of moisture.…”