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Research article2006Peer reviewed

A single-source-precursor approach to late transition metal molybdate materials: The structural role of chelating ligands in the formation of heterometallic heteroleptic alkoxide complexes

Werndrup P, Seisenbaeva GA, Westin G, Persson I, Kessler VG

Abstract

The synthesis and structural determination of three new heterometallic molybdenum complexes, one with cobalt and two with nickel and two of these with beta-diketonate ligands and one with amino alcohol ligands, are presented. The reaction of cobalt acetylacetonate with [MoO(OMe)(4)] provides [Co2Mo2O2(acac)(2)(OMe)(10)] (1) and [MoO(acac)(OMe)(3)] (4), and the reaction of nickel acetylacetonate with [MoO(OMe)(4)] provides [Ni2Mo2O2(acac)(2)(OMe)(10)] (2) and 4. The reaction of [Ni(ORN)(2)] (R-N = CHMeCH2NMe2) with [MoO(OMe)(4)] yields [Ni2Mo2O2(ORN)(2)(OMe)(10)] (3). The two new oxomolybdenum complexes undergo ether elimination upon storage to give the corresponding dioxo complexes [MoO2(acac)(OMe)](2) (5) and [MoO2(ORN) (OMe)](2) (6). Compounds 3 and 4 could also be obtained from the reaction of'stoichiometric amounts of Hacac with [MoO(OMe)(4)] and [MoO2(OMe)(2)], respectively. The local structure around the nickel atom in compound 2 in solution and compound 3 in the solid state and in toluene/hexane solution has been determined by means of EXAFS spectroscopy. The complexes are intended to be used as single-source precursors, which are attractive in coatings and for the preparation of mesoporous materials; its application for the synthesis of nickel molybdate by sol-gel processing is therefore reported. The oxide material obtained from 3 displays a uniform grain size and a large surface area. ((c) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006)

Published in

European Journal of Inorganic Chemistry
2006, number: 7, pages: 1413-1422 Publisher: WILEY-V C H VERLAG GMBH