Nano-NiO catalyzed acylation of mixed (methyl)(aryl)zincs with aromatic acyl halides in THE at room temperature provides a new facile route for aryl-aroyl coupling. Among NiCl2 center dot L-2 and NiCl2 center dot L (L = monodentate and bidentate phosphine ligand) catalysts, the lower catalyst loading of NiCl2 (dppf) may seem attractive; however, nano-NiO, being the lowest cost catalyst, is more favorable for aroylation of (methyl)(aryl)zincs. This procedure also provides a supplement to Cu and Pd catalyzed acylation of diorganozincs.