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Under anaerobic conditions, the reactions of cobalt(II) and nickel(II) acetate tetrahydrate with 2,6‐pyridinedimethanol (H2L2, 3) in anhydrous acetonitrile afforded two tetranuclear metal(II) complexes [MII4(HL2)4(OAc)4] (4; MII = Co2+, Ni2+) with a [M4(μ3‐O)4]4+ cubane core. X‐ray structural analyses revealed that both MII cubanes 4a·2CH3OH and 4b·2CH3OH are isostructural and crystallize in the tetragonal...
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