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Schiff' bases and their transition metal complexes possess a number of biological applications. Metal complexes show higher activity than free ligands. The cobalt complexes shows bright path towards pharmaceutical as well as chemical sciences. In this chapter, we presented the results of synthesis and characterization studies for the three Schiff's base transition metal complexes involving Schiff's base and pseudo halide ligands. The adopted approaches for synthesis of metal complexes are self-assembly method. The IR spectra the existence of functional groups and anionic ligands such as O-H (water), C=C, C=N,N3, NCS, NCO frequencies. The UV spectrum approves the complexation of metal and ligand with the increase in the absorbance value compared to free ligand. The maxvalues of d-d band are detected to be in the range of 300 to 321 nm.The LC-MS spectra predicts the structures of the reported complexes and the m/z values are reported for each fragment of the complex and they confirm the final structure. The TGA determines the breakdown rates of ligands such as H2O, Schiff's base.The results of thermo chemistry are in agreement with the structure of the complexes.