An ammonium tetrathiomolybdate (ATTM) catalyst precursor is synthesized and then thermally decomposed at different temperatures in N-2 or H-2 atmosphere. Characterization of the resulting compounds by powder X-ray diffraction (XRD) and surface area analysis indicates the formation of MoS2-2H with a surface area of 5-9 m(2)/g. When ATTM is treated with cetyltrimethylammonium chloride and then decomposed in N-2 at 723 K, the resulting material has a surface area nearing 200 m(2)/g. If treatment also includes hydrazine, the surface area of the resulting MoS2-2H reaches 215 m(2)/g. Analysis by XRD and electron microscopy shows a noticeable dispersion in the layers of the resulting MoS2. The catalytic activity of the materials is tested in a batch reactor for cyclohexene hydrogenation, where the highest activity sulfides are those obtained by thermal decomposition of the chemically treated precursors in N-2.