Nanorods of Sb2Se3 have been produced from a newly designed single-source precursor under assistance of ethylene glycol used as solvent without any surfactants or additives. The precursor, [(SbL2Cl2)Cl](2)center dot(CH3)(2)CO, 1 (L represents N, N-dimethyl selenourea)], has been easily synthesized and characterized by single crystal X-ray diffraction and IR spectroscopy. The extensive network of NH-Cl bonds present in the crystal packing of the complex promoted the formation of Sb2Se3, leaving HCl in the reaction medium. The Sb2Se3 nanocompounds have been characterized by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM). The mechanism of formation of Sb2Se3 has been proposed and rationalized on the basis of TEM and field emission scanning electron microscopy (FE-SEM) observations of the intermediates throughout the solvent-assisted growth and mass spectral analysis of the reaction mixture during the process