3-Hydroxy-3-p-tolyl-1-m-nitrophenyltriazene and its complex with Iron (III) were synthesized and characterized using several physical techniques like elemental and spectral analysis and their antifungal activity was screened. It was observed that 3- hydroxy-3-p-tolyl-1-mnitrophenyltriazene and its complex with iron (III) showed inhibitory activity at 100 ppm against 3 fungi; Rhizoctonia Solani, Fusarium Solani and Pythium Aphanidermatum. Thus the study has brought about a novel application of this class of analytical reagents as an emerging class of bioactive chemicals