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Tris(N-(pyrrol-2-ylmethyl)-N-butyldithiocarbamato-S,S?)cobalt(III) (1), bis(N-methylferrocenyl-N-(2-phenylethyl)dithiocarbamato-S,S?)nickel(II) (2) complexes were used as single source precursors for the preparation of cobalt sulfide and cobalt-iron sulfide nanoparticles. Morphological characterization of nanoparticles was carried out using TEM and the optical properties by UV-Vis and photoluminescence spectroscopic techniques. The elemental compositions of the nanoparticles were confirmed by energy dispersive X-ray spectroscopy. IR spectral studies on nanoparticles confirm the presence of capping agent (triethylenetetramine).