New iron (III) complexes of S-methyl-βN-(5-methylpyrazole-3-yl) methylenedithiocarbazate, S-benzyl-β-N-β-(5-methylpyrazole-3-yl) methylenedithiocarbazate, 5-methyl-3-formylpyrazole-3- pyrrolidinylthiosemicarbazone, and 5-methyl-3-formylpyrazole- 4N-benzylthiosemicarbazone have been synthesized and physicochemically characterized by elemental analyses, magnetic moment measurements (polycrystalline state), electronic, IR, and EPR spectra, as well as conductance measurements, are used to confirm the coordination geometry. The spectral studies reveal the low-spin distorted octahedral structure of the iron (III) complexes containing two uninegative tridentate ligands with NNS donor sites, where the EPR data confirm the presence of a spin - paired iron (III) with d xz 2 d yz 2 d xy 1 configuration in the ground state. © 2009 Pleiades Publishing, Ltd.