Nickel NPs (< 2 nm) were confined in highly porous metal organic framework (MOF; here, MIL-101(Cr)) via a facile strategy at ambient conditions. With the characterization of HRTEM, XRD, N-2 physisorption, SEM, XPS, TPR, FT-IR, NH3-TPD, ICP-OES, and TG-DTG, the resulting nickel NPs up to 20 Wt% first-ever were detected to be uniformly dispersed, smaller in size and easily reducible in MIL-101(Cr) cages retaining their original crystal structure. The efficiencies of the new sorberits in adsorptive removal of thiophene were investigated. Compared with pristihe MIL-101, the capacity of sulfur adsorption of modified MIL-101 enhanced for thiophene, and obey the order 2ONi-MIL-101 > 10Ni-MIL-101 > 30NiMIL-101 > MIL-101. The improved adsorption properties were linked with surface chemistry and texture of MIL-101 support. Pseudo second-order kinetic and Langmuir models showed best fit Of thiophene adsorption on MIL-101 and Ni-containing MIL-101 samples. Moreover, the rate controlling step for thiophene adsorption was intraparticle diffusion. (C) 2017 Elsevier B.V. All rights reserved.