The main goal of our work was the synthesis and characterization of ZnS(aminopropane) n hybrid inorganicorganic layered materials. The basic material of our investigation was ZnS(1,3-dap) 1/2 , (where dap denotes diaminopropane). Its crystal structure has been solved by X-ray powder diffraction methods. This layered compound was prepared using 1,3-diaminepropane, zinc sulphate (ZnSO 4 ) and tioacetamide (CH 3 CSNH 2 ). We have also tried to obtain and characterize other materials: ZnS(1-ap) and ZnS(1,2-dap), where ap denotes aminopropane. But in these last two cases diffraction patterns were of much poorer quality, which prevented a full structural survey; thus we cannot directly prove that hybrid lamellar materials were obtained. All compounds were studied using X-ray diffraction, chemical analysis, UV-vis spectroscopy and scanning electron microscopy. Additionally, using X-ray diffraction as a function of temperature, we obtained information about structural changes of obtained composite materials under temperature treatment.