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A new series of mononuclear copper (II) and Nickel (II) Schiff base complexes was synthesized and characterized with various techniques like UV, IR, EPR, Cyclic voltammetry studies. The analytical and spectral data obtained are proposed for the complex structures. Copper (II) and Nickel (II) complexes have distorble square-planar geometry around the central metal atom. The synthesized macro cyclic mononuclear copper (II) and Nickel (II) complexes showed good antimicrobial activities the antibacterial. Absorption studies revealed that both Copper and Nickel complexes have pi pi_ and n pi _ transition of important CH=N, C- O and-CH3 functional groups. Electrochemical properties of both complexes were identified by cyclic voltammetry irreversible waves are detected. Antimicrobial studies of Cu (II) and Ni (II) complexes were also been studied. Among seven types of bacteria, v. cholera showed higher long effect of the Copper (II) complex with good inhibition effect towards all bacteria.