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Abstract The overall work is focused on the synthesis of Cu(II), Ni(II), Pd(II), Ru(II) and Rh(III) complexes of 3-(phenylazo)4-hydroxy coumarin and its derivatives, their structures have been elucidated by elemental analysis, IR, UV-vis, ESR, magnetic and conductivity. Square-planar and octahedral are the proposed structures for these complexes. The electrochemical behaviour of the ligands and their complexes was investigated showing that, the peak couples of the ligands attributed to the oxidation of the phenolic hydroxyl to quinine, while the electrode couples of the prepared complexes were found to have ∆Ep> 60 mV and the ip,c vs. ν1/2 plots were linear confirming an irreversible one electron process. The dependence of the cathodic peak current, ip,c and the cathodic peak potential, Ep,c on the scan rate suggests diffused-controlled electrochemical process and ECE mechanism in which an irreversible chemical reaction is interposed between two successive one electron charge transfer. |