We report, herein, the catalytic efficiency and activity of a facilely synthesized sulfided NiMo hydrodesulfurization (HDS) catalyst supported on (Zr)-SBA-15 by one-step calcination and reduction heat treatment prior to sulfidation. Zr-SBA-15-Mo is prepared by a direct synthesis approach, followed by the confinement of Ni into the as-synthesized Zr-SBA-15-Mo without calcination, to generate more dispersion and active sites of metal oxides for an efficient sulfidation process. The HDS performance of these catalysts was evaluated and compared to that of the catalysts prepared by the sequential calcination and reduction approach prior to sulfidation for HDS of dibenzothiophene (DBT) and dimethyldibenzothiophene (DMDBT) in commercial diesel at 350 degrees C in batch reactor mode. Structural and morphological properties related to catalytic activity have been obtained by means of spectroscopy (X-ray diffraction (XRD), Raman, pyridine-Fourier transform infrared (FTIR), temperature-programmed desorption (TPD), microscopy (scanning electron microscopy)), and N-2 physisorption. The characterization and investigations from XRD, Raman, pyridine-FTIR, and TPD revealed that avoiding multiple heat treatment in designing HDS catalysts provides more coordinative unsaturated active sites necessary for better catalyst performance and stability. In addition, the textural properties (specific surface area, pore size, and volume) that allow easy diffusion of reactant molecules are better preserved. The activity of the sulfided NiMo catalysts prepared by one-step heat treatment is 9-16% higher for DBT and 11-13% higher for DMDBT at 1 h reaction time compared to that of the catalysts prepared by sequential calcination and reduction before sulfidation. The catalysts prepared by this heat treatment approach have desulfurization efficiencies of 99 and 84% for DBT and DMDBT, respectively.