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Abstract Three substituted thiosemicarbazides (two mono- and one bis-) were prepared and characterized. Their reactions with cobalt(II), nickel(II), copper(II), zinc(II), iron(III), cadmium(II), oxovanadium(IV) and dioxouranium(VI) ions afforded mononuclear complexes in case of the two mono - ligands and binuclear complexes in case of the bis – ligand. Surprisingly, the bis – ligand afforded mononuclear complexes in case of Zn(II) and VO(IV) with unique modes of bonding. Various geometries were obtained; octahedral; tetrahedral; square planar and square pyramid. Structure elucidation of the ligands and their metal complexes were achieved on the basis of elemental, thermal analyses, conductivity and magnetic susceptibility measurements as well as spectral studies; electronic, vibrational, mass, ESR and 1H-NMR spectra. |