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The work described in this Ph.D. thesis is the outcome of the ideas framed while studying the literature on the development in the area of coordination chemistry. It was aimed to synthesize and characterize some coordination compounds of first row transition metals incorporating the ligands viz., 1,2-diaminophenyl-N,N'-bis-(2-pyridenecarboxaldimine), N,N'-bis-(2-pyridenecarboxaldimine)-1,8-diamino-naphthalene, bis-(thiophene-2-carboxaldimine)-1,8-diaminonaphthalene.