The preparation of a representative series of lead thiolates, Pb(SR)2(R = Et, Bun, But, Ph, p-C6H4Me, o-C6H4Me, p-C6H4Cl), is reported. Thermal decomposition of these thiolates leads to the formation of lead sulphide and the organic sulphide, R2S. Reaction of the thiolates with sulphur (or selenium) gives lead sulphide (or selenide) and the organic disulphide, R2S2. An assessment of the stability of lead thiolates in common organic solvents is given.