Two new Schiff bases have been synthesized by the reaction of p-aminoazobenzene with salicylaldehyde ((LH)-H-1) and the oxidative polycondensation product of (LH)-H-1 ((LH)-H-2,). The complexes of cobalt(II), copper(II), and nickel(II) with (LH)-H-1 and (LH2)-H-2 have been prepared. The ligands and their complexes have been characterized by elemental analyses, IR spectra, electronic absorption spectra, mass spectra, H-1 and C-13 NMR spectra, and magnetic susceptibility measurements. The thermal properties of all complexes have been studied by TG and DTA. The analytical data show that the metal to ligand ratio in the (LH)-H-1 complexes is I : 2. but in the (LH2)-H-2, complexes it is 1 : 1.