The dicompartmental macrocyclic ligand (L2)2- was prepared by [1:1] cyclic condensation of N,N?-dimethyacetate-N,N?-ethylene-di(5-methyl-3-formyl-2-hydroxybenzylamine with 1,3-diaminopropane. The ligand includes dissimilar N(amine)2O2 and N(imine)2O2 coordination sites sharing two phenolic oxygen atoms and containing two methyl acetate pedant arms on the amine nitrogen donor atoms. A series of mono- and bimetallic complexes were synthesized and characterized on the basis of elemental analysis, molar conductance measurement, IR and UV-Vis spectroscopy techniques. It was found that during the cyclization process the copper (II) displaced from the N(amine)2O2 to the N(imine)2O2 coordination site and one of the methyl acetate pedant arms is dissociated. The heterodinuclear complex of [ZnL2Cu(?-OAc)]+ was prepared by a transmetallation reaction on the [ZnL2Zn(?-OAc)]+ by Cu(II). The characterization results showed that the two metal ions are bridged by two phenolic oxygen atoms and an acetate group, providing distorted five-coordination geometries for the both metal ions.