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We synthesized the binuclear Tetradentate Schiff base nickel(Ⅱ) and copper(Ⅱ) complexes ; [Ni(Ⅱ)2(SMPO)2(L)2], [Ni(Ⅱ)2(SPPD)2(L)2] and [Cu(Ⅱ)2(SMPD)2] and [Cu(Ⅱ)2(SPPD)2] (where, L : Py, DMSO and DMF). We identified the structure of these complexes by elemental analysis, IR-spectrum, T.G.A, D.S.C and ESR measurements. According to the results of cyclic voltammetry and DPP measurements in aprotic solvent included 0.1M TEAP as supporting electrolyte, we knew that diffusional controlled redox process of one step with one electron was irreversible process in 0.1M TEAP-Py solution. Also it was reversible or quasi reversible process in 0.1M TEAP-DMSO solution and reversible or E.C reaction mechanism in 0.1M TEAP-DMF solution at mononuclear complexes ; [Cu(Ⅱ)(SOPD)] and [Ni(Ⅱ)(SOPD)(L)2]. But, we knew that diffusional controlled redox process of two step for one electron of binuclear complexes was as follows. The values of redox potential for dimeric complexes in 0.1M TEAP-L solution (where, L ; Py, DMSO and DMF) with scan rate 100mV/sec.
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