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An investigation of the solid-state X-ray structure of the new organic–inorganic compound [C5H14N2]2PbCl6·3H2O shows a layered organization of the (PbCl6)4– anions, with (R2NH2)+ groups and water molecules developed in the [001] plane at x = (2n + 1)/4. The crystal structure is stabilized by N − H···Cl, N − H···O, O − H···Cl, O − H···O, and C − H···Cl hydrogen bonds. The powder X-ray diffraction and X-ray photoelectron spectroscopic (XPS) analyses confirm the phase purity of the crystal sample. The intermolecular contacts are quantified using the Hirshfeld surfaces computational method. The major inter-contacts contributing to the Hirshfeld surfaces are H...Cl, H...H, and O...H. The vibrational modes were identified and assigned by IR and Raman spectroscopies. The optical properties were investigated by UV–visible and photoluminescence spectroscopic studies. The compound was characterized by thermal analysis to determine its thermal behavior with respect to the temperature. Finally, X-ray photoelectron spectroscopy analysis is reported for analyzing the surface chemistry of [C5H14N2]2PbCl6·3H2O. [ABSTRACT FROM AUTHOR]