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In order to develop a novel model to predict if a so called normal tetrahedral compound crystallizes in a  wurtzite - or  sphalerite  superstructure type, the system Cu 3 AsS 4 –Cu 3 SbS 4  was reinvestigated. A solid solution series was prepared and the mixed crystals were characterized by powder X-ray techniques. The crystal structures of Cu 3 As 0.330 Sb 0.670 S 4 , Cu 3 As 0.736 Sb 0.264 S 4 , and Cu 3 AsS 4  were refined from single crystal X-ray data. The refinements converged to  R  = 0.0209,  wR 2 = 0.0484 (Cu 3 As 0.330 Sb 0.670 S 4 , 201 unique reflections, 15 parameters),  R  = 0.0235,  wR 2 = 0.0596 (Cu 3 As 0.736 Sb 0.264 S 4 , 218 reflections, 15 parameters), and  R  = 0.0241,  wR 2 = 0.0669 (Cu 3 AsS 4 , 721 reflections, 45 parameters).  Z  is 2 for all compounds. The volumes of the tetrahedra [MS 4 ] were calculated for the investigated compounds. In addition, the corresponding data were calculated for further solids from literature data. The volumes of the tetrahedra are used to separate compounds with a  sphalerite  type anion arrangement from compounds with hexagonal packed anions. A closer inspection of the tetrahedra volumes reveals a greater variation for one given material in the case of  wurtzite  type superstructures than for  sphalerite  type superstructures. A critical difference in the tetrahedra volumes is derived from these data.

The system Cu 3 AsS 4 –Cu 3 SbS 4 and investigations on normal tetrahedral structures