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Single-layer, ultrasmall ReS2 nanoplates embedded in amorphous carbon were synthesized from a hydrothermal treatment involving ammonium perrhenate, thiourea, tetraoctylammonium bromide, and further annealing. The rhenium disulfide, obtained as a low dimensional carbon composite (ReS2/C), was tested in the hydrodesulfurization of light hydrocarbons, using 3-methylthiophene as the model molecule, and showed enhanced catalytic activity in comparison with a sulfide CoMo/-Al2O3 catalyst. The ReS2/C composite was characterized by X-ray diffraction (XRD), Raman spectroscopy, N2 adsorption-desorption isotherms, scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). The improved catalytic performance of this ReS2/C composite may be ascribed to the presence of a non-stoichiometric sulfur species (ReS2-x), the absence of stacking along the c-axis, and the ultra-small basal planes, which offer a higher proportion of structural sulfur defects at the edge of the layers, known as a critical parameter for hydrodesulfurization catalytic processes. [ABSTRACT FROM AUTHOR]