4-Formylantipyrine N(4)-antipyrinylthiosemicarbazone and its metal complexes have been synthesized and characterized. Elemental analyses, molar conductivities, magnetic measurements and spectral (i.r., electronic, n.m.r., e.s.r.) studies have been used to characterize the complexes. The i.r. spectra show that the thiosemicarbazones behave as bidentate (NS) or tridentate ligands (ONS), either in the thione or thiolato form. Stereochemistries are proposed for the complexes on the basis of both spectral and magnetic studies.