Abstract. Single crystals of Zn 1−x MnxIn 2 Se 4 were grown by the chemical vapour phase transport (CVT) technique. Through X-rays powder diffraction patterns and Laue diagrams of single crystals we studied the transformation from the layered rhombohedral structure of MnIn 2 Se 4 to the tetragonal structure of ZnIn 2 Se 4 . On the ZnIn 2 Se 4 side, we observe single-phase, solid solution samples for x=0.01 and x=0.25, as is the case for the MnIn 2 Se 4 side with x=1 and x= 0.87. For the intermediate concentrations x=0.35, x=0.60 and x=0.67 we observe our samples to be two-phase mixtures.