A novel azo dye ligand formed by the coupling of L-histidine with 2-hydroxy-1naphthaldyhide(H 2 L) and its Ru 3+ , Pd 2+ and Ni 2+ nano-sized complexes were obtained and described by elemental analysis, TGA, magnetic moment measurements, molar conductance, UV-Vis, ESR, X-ray powder diffraction, IR, SEM, TEM, 1 H-nmr, 13 C-nmr, and EI-mass spectral studies. The analytical results and spectral studies detected that the H 2 L ligand acts as dibasic tetradentate via aldehyde oxygen, azo nitrogen and deprotonated OH and COOH groups. The data showed the paramagnetic Ru 3+ complex has octahedral geometry while Pd 2+ and Ni 2+ have square planar structures. The molar conductance measurements display all complexes are nonelectrolyte. The crystallinity, morphology and average particle size data revealed the prepared complexes were formed in the Nano scale. The average particle size as calculated from TEM images are found to be 13.72, 64.52 and 115.00 nm for Ru 3+ , Pd 2+ and Ni 2+ chelates, respectively. The catalytic activities of these compounds were checked for oxidation of 2-amino phenol to 2-amino-3Hphenoxazine-3-one as heterogeneous catalysts. A 96, 31 and 21% catalytic conversion are found when using Ru(III), Pd(II) and Ni(II) complexes respectively.