The interaction of Co(acac)2 and Ta(OMe)5 in dry toluene led to formation of crystalline [Co2Ta2(acac)2(OMe)12] 1 and [Ta(acac)(OMe)4] 2 complexes. If the starting material is not completely water-free the products obtained are [Co4(acac)6(OMe)2(MeOH)2] 3 and Co(acac)2·2MeOH 4 due to hydrolysis of Ta(OMe)5 producing free methanol and thus altering the reaction pathway. The interaction of MII(acac)2, MII = Co, Ni, Zn or Mg, and MV(OMe)5, MV = Ta or Nb, in dry toluene was found generally to provide MII2MV2(acac)2(OMe)125–8, a new class of heterometallic heteroleptic alkoxide complexes. The crystal structures of 1–8 have been determined.
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