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In continuation of our previous book the coordination chemistry of new thiosemicarbazides/thiosemicarbazones ligands and its metal complexes were discussed in present project. Some new functionally important thiosemicarbazides/thiosemicarbazones contain S-N donor site in suitable positions were synthesized and characterized on the basis of their physical, elemental and spectral studies. Also the metal complexes of these newly prepared thiosemicarbazone ligands characterized by using elemental analyses, mass spectra and FT-IR spectrum. Further electronic spectral study along with magnetic data was examined to confirm the geometry of metal complexes, while TGA were well discussed for decomposition temperature and degradation pattern. Furthermore, the discovery of antibacterial activities of all synthesized compounds were carried out using several Gram (+) and Gram (-) bacterial strains which suggest that the metal complexes found more active than its free ligand.