In this study, we used the facile solvent evaporation method to achieve the inorganic-organic hybrid crystals of [triethylpropylammonium][PbI], which have been characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and differential scanning calorimetry as well as single-crystal X-ray structure analysis. The hybrid solid crystallizes in the monoclinic space group P2/c at room temperature and is composed of one-dimensional [PbI] chains, where the neighboring PbI coordination octahedra connect together via the face-sharing mode and the organic cations fall in the spaces between [PbI] chains. The hybrid exhibits a dielectric phase transition with a critical temperature of ca.
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