Zinc- and cadmium bis(alkylthiolate) compounds have been prepared and converted into the appropriate binary metal sulfides by thermal treatment. Several mercury chlorothiolates have been synthesized and characterized by single crystal X-ray diffraction. Their decomposition pathways are discussed. The prepared binary metal sulfides have been studied by XRPD and - in selected cases - by particle size determination. The volatile co-products have been isolated and characterized by GC/MS.