The preparation of solid solutions of the sulfides of zinc, cadmium, and lead has been attempted by low-temperature pyrolysis (150-400 degrees C) of metal bis(benzylthiolate) precursors. The (Zn,Cd)S shows solid solution behavior at 200-400 degrees C and crystallite sizes of similar to 5 nm. The CdS-PbS system was also prepared by the precursor decomposition method, exhibiting interesting behavior in the lead-rich region. The 150 degrees C pyrolysis of Pb(SBn)(2) leads to nanocrystalline (20-40 nm) PbS single crystals distributed throughout: the nanocrystalline (similar to 2-5 nm) regions of CdS. Pyrolysis at 200 degrees C produced 40-60 nm PbS cubes dispersed throughout nanocrystalline (similar to 2-5 nm) CdS. The solids produced were characterized by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, selected area electron diffraction, energy-dispersive X-ray analysis, and elemental analysis.