Uniform-sized semiconducting nanocrystals of binary metal sulfides are synthesized from the thermolysis of metal-oleate complexes in alkanethiol. The size of the Cu(2)S nanocrystals can be tuned from 7 to 20 nm by varying the reaction conditions. Various shaped nanocrystals of CdS, ZnS, MnS, and Pb are synthesized from the thermal reaction of metal-oleate in alkanethiol.