The synthesis and characterization of a series of homologous tetranuclear complexes [(iPr3PCu)2(MR2)2(SCH2CH2S)2] (MR2 = GaMe2 (2), GaEt2 (3), GaiPr2 (4), GanBu2 (5) and InMe2 (6), InEt2 (7), IniPr2 (8), InnBu2 (9)) and of related compounds [(iPr3PCu)3(MR2)(SCH2CH2S)2] (MR2 = GaMe2 (10), GaEt2 (11), GaiPr2 (12), GanBu2 (13) and InMe2 (14), InEt2 (15), IniPr2 (16), InnBu2 (17)) are presented. The molecular structures of these were determined by single crystal X-ray diffraction. Thermolysis processes of all the representatives of 2–9 were investigated by simultaneous thermal analysis and thermal decomposition in a nitrogen atmosphere in a quartz glass tube. According to powder X-ray diffraction studies these thermolysis residues predominantly consist of CuMS2 (M = Ga, In), which mainly occurred in the well known tetragonal chalcopyrite-type structure and partially in the hexagonal wurtzite-type structure. As expected from their composition, representatives of 10–17 form mixtures of CuMS2 and large amounts of Cu2−xS upon thermolysis.
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