Single crystals of 3-(4-fluorophenyl)-1-(4-methylphenyl)prop-2-en-1-one (FMPP) have been grown by mixed solvent system ethanol and chloroform 2:1 (v/v) at room temperature. Single crystal X-ray diffraction reveals that FMPP belongs to monoclinic system with four molecules in the unit cell. The structure and the crystallinity of the material were further confirmed by FT-IR, FT-Raman, and powder X-ray diffraction analyses. The band gap energy is estimated by Kubelka-Munk algorithm using DRS data. Theoretical calculations were performed to derive the optimized geometry and the first-order molecular hyperpolarizability (beta) values. The as-grown crystal is further characterized by GC-Mass, SEM, and thermal analyses.