Copper(II) and Nickel(II) complexes of N-substituted Thiosemicarbazide ligands derived from condensation of two thiosemicarbazide and a dicarboxylic acid(malonic/ succinic/phthalic acid) have been synthesized and characterized by elemental and thermal analysis, IR, UV-Vis and EPR spectral studies, and magnetic susceptibility studies. Anti-bacterial, Anti-fungal and Anti-cancer activities have also been carried out on these complexes. Most of the complexes have good antibacterial and antifungal activity and some of them show excellent anticancer activity too.