The synthesis and characterization of two new N₂O₄ donor type ligands, 2-{[(2-{3-[2-({[(2-hydroxyphenyl)methylidene]amino}methyl) phenoxy]propoxy}benzyl)imino]methyl}phenol (H₂L1) and 2-[({2-[3-(2-{[(2-hydroxybenzyl)amino]methyl}phenoxy)propoxy]benzyl}amino) methyl]phenol (H₂L2), and their metal complexes with Cu(II) and Ni(II) metal ions are reported. The ligands and complexes have been characterized by ¹H NMR, FT-IR, UV-Vis absorption spectroscopy, single-crystal X-ray diffraction, CHN elemental analysis and cyclic voltammetry (CV). The redox behavior of the two complexes has been studied by CV. Copper and nickel complexes of Schiff base (H₂L1) and reduced Schiff base (H₂L2) showed different behaviors because the structure of the complexes depends of the ligand. The complex [Cu₂L1 ₂]·2CH₃OH (1) is dinuclear with the two metal centers bridged exclusively by the ligands, consisting of two distorted square planar CuN₂O₂ chromophors with large intermetallic separation (8.879 Å). Complex [Ni₄L2₂(CH ₃COO)₄]·4CH₃OH (2) consists of tetranuclear Ni₄ unit of two symmetry related hexacoordinated nickel atoms having distorted octahedral NiN₂O₄ and NiO ₆ environments, and contains two types of acetate coordination modes, namely, bridging bidentate (μ₂-η¹, η¹), and asymmetric chelating bridging (μ₂- η², η¹).