Molybdenum(IV) disulfide was prepared by the thermalysis of the single molecule precursor [Mo2O4(S2C- NEt2)(2)] (Et: ethyl group). The thermalysis was monitored by thermogravimetric analysis and FT-infrared spectroscopy. The MoS2 materials obtained during the thermalysis experiments were characterized in terms of their morphological and optical characteristics. (C) 2003 Elsevier Ltd. All rights reserved.