Schiff base ligands have been in the chemistry catalogue for over 150 years. Schiff bases are typically formed by condensation of primary amine and an (aldehyde/Ketone). The resulting compound R 1 R 2 C=NR 3 is called Shiff base.Shiff bases are generally bidentate, tridentate, tetradentate or polydentate.ligands capable of forming very stable complexes with transition metals. These compounds play an important role in the coordination chemistry related to catalysis and enzymatic reactions, magnetism and molecular architectures. Interest in the design, synthesis and characterization of transition metal complexes of unsymmetrical Schiff base ligands stems from the fact that the central metal ions in natural systems are unsymmetrical. Such compounds have been suggested as useful probes for the study of low symmetry complexes related to the low symmetry sites found in metalloproteins. These complexes are valuable to theoretical and experimental chemists, as the steric and electronic factors of the Schiff base can be tuned systematically by introducing suitable substituents to bring about subtle structural variations that are extremely useful to deduce a relation between magnetic coupling and structural features .Recently, this , one of the major problems which is commonly encountered is the hydrolysis process which leads to hydrolytic rearrangements of the Schiff base. On this basis, in this thesis a new ligand, H 2 Bzacabzanapht, and its metal complexes, which may have biochemical and photochemical applications, are synthesized, characterized and studied 4.[Ni(Bzacabzanapht)] 1. [Mn III (Bzacabzanapht)N 3 ] n 5. [Cu(Bzacabzanapht)] 2. [Mn III (Bzacabzanapht)SCN] 3.[Fe III (naphtabza)Cl] . The complexe [Fe III (Bzacabzanapht)] has been found to rearrange into the more symmetrical complexe [Fe III (naphtabza)], a phenomena attributed to the concurrent presense of Fe +3 and Cl - . The H 2 Bzacabzanapht and its complexes were characterized by UV-Vis, FT-IR, 1 H-NMR, elemental analysis.The ligand and complexes (1), (3), (4), (5) were structurally characterized by X-Ray diffraction. The electrochemical properties of the compounds were also studied using cyclic voltammetry.