NiMo catalysts were prepared using Waugh-type NiMo heteropolycompounds as active phase precursors and evaluated in hydrodesulfurization (HDS) of dibenzothiophene (DBT). These catalysts were compared with corresponding reference catalysts prepared from the conventional precursors (ammonium heptamolybdate and nickel nitrate). Prepared catalysts were characterized by N-2 physisorption, XRD, FT-IR, H-2-TPR, DRIFT of CO adsorption and HRTEM techniques. It was found that NiMo catalysts prepared from Waugh-type NiMo HPCs showed higher performance in HDS of DBT than their counterparts. Possible reasons of this result were discussed.