Thiosemicarbazones are versatile ligands of considerable significance with respect to their variable coordination behavior, biological properties, physico-chemical properties of also catalytic activity of their transition metal complexes.1,2 For instance, some iron(III) complexes of thiosemicarbazone-based ligands show antitumor activity by inhibiting ribonucleotide diphosphate reductase.3 Moreover, to date a number of colorimetric and also fluorescent receptors based on thiosemicarbazone have been reported which are capable to detect transition metal ions in organic and aqueous media.3 We report here synthesis and characterization of a new unsymmetric thiosemicarbazone-based azo-azomethine ligand, H2L, by condensation reaction of an ethyl derivative of azo coupled thiosemicarbazide with 4-chloro-2-amino phenol in ethanol. The prepared ligand was characterized using NMR, IR and UV-Vis spectroscopic methods as well as Mass spectroscopic data. Furthermore, a new Fe(III) complex was also prepared via direct reaction of H2L with FeCl3 in ethanol. The resultant complex was identified via IR and UV-Vis spectroscopy aswell as elemental analysis.