We report a facile chemical route for the synthesis of monodisperse nanocrystals of various metal sulfides (PbS, Cu2S, and Ag2S) and their assemblies into nanocrystal superlattices (NCSs); the sulfides NCSs were precipitated by adding ethanol to nanocrystal colloids, which were obtained directly by a reaction between metal thiolate and thioacetamide in a pure dodecanethiol solvent.