New complexes of Co(II), Ni(II), Cu(II), and Zn(II) with new Schiff bases derived by the condensation of p -aminoacetophenoneoxime with 5-methoxysalicylaldehyde are synthesized. The compounds are characterized by elemental analyses, magnetic susceptibility measurements, IR, 1 H and 13 C NMR spectra, electronic spectral data, and molar conductivity. The thermal stabilities of the compounds are also reported. The Schiff base acts as bidentate O,N-donor atoms, and their metal complexes are supposed to possess a tetrahedral geometry with respect to the central metal ion. The general formula of the 5-methoxysalicyliden-p -aminoacetophenoneoxime Co(II), Ni(II), Cu(II), and Zn(II) complexes is Co(L) 2 , Ni(L) 2 , Cu(L) 2 , and Zn(L) 2 .