Ni°-nanoparticles of 0–8nm were prepared in situ by impregnation of Ni(CH 3 COO) 2 into the nanopores of modified montmorillonite (Mt) followed by polyol reduction. The Mt was activated with HCl under controlled condition for generating desired pore sizes. The porous materials were characterized by XRD, TEM, SEM, UV–visible spectroscopy, FTIR and XPS analysis. N 2 adsorption data revealed specific surface areas (BET) in the range of 296–548m 2 /g, specific pore volumes of 0.4–0.6cm 3 /g and pore diameters of 0–6.8nm. XRD pattern of Ni°-nanoparticles revealed the formation of face centered cubic (fcc) lattice. These supported Ni o -nanoparticles show efficient catalytic activity in transfer hydrogenation of acetophenone to 1-phenylethanol with about 98% conversion, having nearly 100% selectivity.