In this study, the new Schiff base ligands N,N′-bis[(1Z,2E)-1-(4-methylphenyl)-2-(hydroxyimino)-1-phenylethylidene]-4-methylbenzene-1,2-diamine and N,N′-bis[(1Z,2E)-1-(4-chlorophenyl)-2-(hydroxyimino)ethylidene]-4-methylbenzene-1,2 diamine have been synthesized. Their metal complexes with copper and nickel have been formed and characterized by FT-IR, UV-Vis, NMR, LC/MS-MS spectra, molar conductivity, magnetic susceptibility, elemental analysis, ICP-OES, and thermogravimetric analysis. The complexes demonstrate semiconducting features.