A cationic molybdenum sulfide cluster [Mo3S4(H2O)(9)](4+) with incomplete cubane-type structure and a cationic nickel-molybdenum mixed sulfide cluster [Mo3NiS4Cl(H2O)(9)](3+) With complete cubane-type structure were introduced into zeolites NaY, HUSY and KL by ion exchange. Stoichometry of the ion exchange was well established by elemental analyses. The UV-visible spectra and EXAFS analysis data exhibited that the structure of the molybdenum cluster remained virtually intact after ion exchange. MoNi/NaY catalyst prepared using the molybdenum-nickel sulfide cluster was found to be active and selective for benzothiophene hydrodesulfurization.