Organic-inorganic hybrid materials of the type MeQ(diamine)(1/2) (where Me-Zn, Cd, Mn and Q-S, Se, Te) belong to the class of 3D nanomaterials. They are built of layers of II-VI semiconductors and amines, which act as linkers. The main goal of our work was the synthesis of compounds of the type ZnxCd1-xSe(1,3-diaminopropane)(1/2) and ZnSySe1-y(1,3-diaminoPrOPane)(1/2) (where x, y = 0, 0.25, 0.5, 0.75, 1) and the study of properties changed by the composition of the semiconducting layers. Analysis of these materials was carried out with the use of X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC) as well as temperature dependent XRPD enabled us to obtain information about the thermal stability of hybrid compounds with mixed semiconducting layers. Another important part of our work was a study, performed with the use of UV-vis spectroscopy, of the optical properties of these materials.