In this thesis a new ligand, H 2 Me-salabza, and its metal complexes: (1) [Cu II (Me-salabza)] (3) [Co III (Me-salabza)(py) 2 ]PF 6 (2) [Ni II (Me-salabza)] (4) [Co III (Me-salabza)(3-Mepy) 2 ]PF 6 (5) [Co III (Me-salabza)(bzlan) 2 ]BPh 4 Were synthesized, characterized and studied. Complexes 1-5 were synthesized in good yield and characterized via FT-IR, UV-Vis , 1 HNMR and CHN analysis. The electrochemical properties of the compounds were studied using Cyclic Voltammetery and a good correlation was found between the spectral and electrochemical properties of these complexes. The electron donation properties of Me-salabza were compared with those of salabza using the electrochemical data. In Cobalt complexes, The correlaton of electrochemical properties with the axial ligand were studied. It was observed that the rodeox properties of the Co(III) complex is irreversible, and is dependent on the electron donating strength of the axial ligand.