An approach to heterometallic alkoxide-beta-diketonate complexes with a M4O4 cubane-like core and new prospects of their application in preparation of solid catalysts. X-ray single crystal study of (Co,Ni)(4)(acac)(4)(mu(3)-OMe)(4)(MeOH)(4), Co2Ni2(acac)(4)(mu(3)-OMe)(4)(OAc)(2) and Mg-4(acac)(4)(mu(3)-OMe)(4)(MeOH)(4)

The interaction of the individual M-4(acac)(4)(mu (3)-OMe)(4)(MeOH)(4) comp lexes, M = Co, Ni in toluene;methanol media provided crystals of (Co,Ni)(4) (acac)(4)(mu (3)-OMe)(4)( MeOH)(4) (I) - the product of co-crystallization of isomorphous products. The oxidation of a MeOH solution of I in air in th e presence of NaOAc and aminoalcohols as catalysts gave Co2Ni2(acac)(4)(mu (3)-OMe)(4)(OAc)(2) (II), an individual heterometallic derivative. The inte raction of Mg(OCH(CH3)CH2NMe2)(2) with Cu(acac)(2) in toluene/methanol medi a produced Mg-4( acac)(4)(mu (3)-Me)(4)( MeOH)(4) (III) as the only isolata ble product. The starting Co and Ni homometallic complexes as well as the h eterometallic CoNi complex II were used to prepare the zeolite-supported ox ide catalysts which exhibited extremely high activity towards methanol oxid ation. (C) 2001 Elsevier Science Ltd. All rights reserved.