The present work describes facile synthesis of a novel Fe(acac)3 decorated g‐C3N4 heterostructure. Mixing of iron(III) complex with g‐C3N4 thorough simple ultrasonication leads to the formation of the heterostructure. The material was thoroughly characterized by FT‐IR, powder XRD, SEM, TEM, UV/Vis DRS and XPS analysis. The analytical results clearly indicate that the FeIII complex is uniformly interspersed with g‐C3N4. The results also suggest that there exists synergy between two components in the heterostructure for enhance catalytic performance. This novel material was used as heterogeneous catalyst for visible light driven oxidation of a number of alcohols by H2O2. The best ratio of the Fe(acac)3 and g‐C3N4 is determined with PL analysis. Cold LED light was used as source of visible light. Metal complex decorated g‐C3N4 heterostructured materials have been rarely used as catalysts for synthetically useful organic transformations. Thus present work on the use of this materials promises to open up new avenues in future growth in metal complex‐graphitic nitride based heterostructure nanocatalysis.