Four new mixed ligand complexes Me(II)/phenylalanine (phe)/HL [HL =4-(4-bromophenyl- aminoisonitrosoacetyl)biphenyl and Me = Co, Ni, Cu, Zn] were synthesized. These complexes are formulated as: [CoL(phe)(H2O)2], [NiL(phe)(H2O)2], [CuL(phe)(H2O)2] and [ZnL(phe)(H2O)2]. All the compounds were characterized by elemental analyses, FT-IR, magnetic susceptibility measurements, TG/DTA and cyclic voltammetry (CV) experiments. IR spectral data confirmed the coordination of the oxime ligand to the metal ions through the oxime and carbonyl oxygen. The geometrical structures of the complexes have been found to be octahedral. The measured molar conductance values of the complexes in DMF are in agreement with the non-electrolytic nature ofthe complexes. The elemental analyses confirm a 1:1:1 [metal:HL:L(phenylalanine)] molar ratio. Thermal behavior of the compound was investigated by thermal gravimetric analysis (TG) and differential thermal analysis (DTA) techniques. All the complexes were transformed into metal oxides after thermal degradation. The electrochemical properties of both ligand and their complexes were analyzed by cyclic voltammetry (CV) using glassy carbon electrode in DMF solution containing 0.1 M TBAP as supporting electrolyte.                     KEY WORDS: Oxime, electrochemical characterization, mixed ligand complexes, amino acid, phenylalanine   Bull. Chem. Soc. Ethiop. 2020, 34(3), 543-556. DOI: https://dx.doi.org/10.4314/bcse.v34i3.10