The relation between structure and electrochemical reactivity underlie the participation of transition metals in many important processes including catalysis, energy conversion, and biological electron transfer. In this thesis, with the goal of evaluating the structural effects on the electrochemical properties of first row d block transition metal complexes, the cyclic voltammetry of a large number of schiff base and carboxamide complexes of Cu(II), Ni(II), Co(III), Zn(II) and Cd(II) has been studied. It has been found, that the electron density on the metal center, is not only dependent on the electronic parameters of the donor atoms of the ligands but the structural and steric parameters also play an important role on the redox properties of metal center. An electrerochemical series for the studied Schiff base and carboxamide ligands is also presented.