The synthesis and characterization of nickel(II) and zinc-(II) complexes with 4-formylantipyrine N(4)-methyl-, N(4)-dimethyl- and 3-piperidylthiosemicarbazones are reported. Elemental analyses, molar conductivities, magnetic measurements and spectral (i.r., electronic and n.m.r.) studies have been used to characterize the complexes. The i.r. spectra show that the thiosemicarbazones behave as bidentate or tridentate ligands, either in the thione or thiolato form. Stereochemistries are proposed for the complexes on the basis of spectral and magnetic studies.