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Copper and cobalt complexes derived from 3-(N-phenyl)-thiourea-pentanone-2 were characterized by elemental, XRD, FTIR, UV-Vis, SEM and 1H NMR spectroanalytical studies. The X-ray diffraction studies indicate that 3-(N-phenyl)-thiourea-pentanone-2 and complexes with copper and cobalt are crystalline in nature with simple cubic lattice structure. IR spectroscopic data were used to assign characteristic vibrational frequencies of groups present in these compounds. Scanning electron micrograms were used to assign morphology and particle size.