The Ni(II) complexes [Ni(L) 2 ](ClO 4 ) 2 (1) and [Ni(L) 2 (NO 3 ) 2 ] (2), where L is the Schiff base ligand of 4,5,9,13,14-pentaaza-benzo[b] triphenylene, were synthesized and characterized by physico-chemical and spectroscopic methods. Nano-sized particles of (1) were prepared both by sonochemistry (3) and solvothermal (4) methods. NiO nanoparticles were obtained by calcination of the nano-structure complexes at 500°C. The structures of the nano-sized compounds were characterized by X-ray powder diffraction and scanning electron microscopy. The thermal stabilities of the bulk complexes (1-2) and nano-sized particles (3-4) were studied by thermogravimetric and differential scanning calorimetry. The catalytic activities of complexes of (1-4) are reported. The free Schiff base and its Ni(II) complexes have been screened for antibacterial activities against three Gram-positive bacteria. The metal complexes are more active than the free Schiff base. Electrochemical studies show that the Ni complexes undergo irreversible reduction in MeCN solution.