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One new hexanuclear Cu(II) complex [Cu 4 (L 1 ) 4 Na 2 (ClO 4 )(H 2 O)](ClO 4 )(H 2 O) 0.5 ( 1 ) and two new tetranuclear Ni(II) complexes [Ni 4 (L 2 ) 4 (CH 3 OH) 4 ] ( 2 ), [Ni 4 (o-vanillinate) 4 (μ 3 -N 3 ) 4 (CH 3 OH) 4 ] ( 3 ) have been synthesized and structurally characterized. All the three complexes 1 , 2 , and 3 have been characterized by elemental analysis, FTIR, and single crystal X-ray diffraction studies. Single crystal X-ray diffraction studies reveal that all three complexes consist of a cubane core in which the four Cu(II)/Ni(II) centers in 1 and 2 are linked by μ 3 -alkoxo bridges and Ni(II) ions in 3 are linked by azido bridge in end-on fashion. The skeleton structures of the cubane cores are all distorted from the idealized cube and most show a further distortion. The variable-temperature (2–300 K) magnetic susceptibilities and magnetizations of the three compounds were measured. Variable-temperature magnetic susceptibility data exhibit dominant antiferromagnetic interaction in complex 1 while ferromagnetic interactions in complexes 2 and 3 . [ABSTRACT FROM AUTHOR]