—A series of N-morpholine or N,N-diethyl, N'-substituted benzoylthioureas (R = Cl, Br, OMe or NO2 in ortho-, meta- or para-position) has been synthesized by condensation of morpholine or diethylamine with substituted benzoyl isothiocyanates. NMR spectra and magnetic measurements have shown square-planar NiL2 and fac-CoL3 complexes. The influence of the different substituents on the NMR and electronic