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A new organic-inorganic crystal, N-(2-ammonium ethyl)-propane-1,3diammonium hexachlorobismuthate(III) has been synthesized by the slow evaporation method at room temperature and characterized by X-ray diffraction, thermal analyse (DSC), spectroscopic FT-IR and Raman. The single X-ray diffraction studies have revealed that the compound crystallizes in monoclinic non-centrosymmetric space group Pn, the crystal is built up of separated  octahedral anions and N-(2-ammonium ethyl)-propane-1,3diammonium cations. The cohesion of the structure is achieved by an extensive network of N–H…Cl hydrogen bonds between the N-(2-ammonium ethyl)-propane-1,3diammonium cations and the octahedra  anions, in which they may be effective in the stabilization of the crystal structure. Differential scanning calorimetry (DSC) disclosed structural phase transition of the order-disorder type at 398K. The Raman studies of the polycrystalline  performed in the frequency region between  and  show that the vibrational state of N-(2-ammonium ethyl)-propane-1,3diammonium cation does not change around the phase transition point. 

organic-inorganic hybrid material, DSC, phase transition, IR absorption, Raman scattering.