L-valinium picrate, an organic material, was synthesized and grown by solution growth method. Cell parameters of the grown crystals were obtained from the single crystal X-ray diffraction analysis and the presence of functional groups was identified by FTIR study. The quality of the crystal was also examined by high-resolution X-ray diffraction study. Its optical properties were examined by UV-Vis-NIR analysis, which shows that the crystal is transparent between the wavelengths 400 and 1000 nm. Thermal analysis carried out for the L-valinium picrate exhibits a single sharp melting point at 269 °C. The Vicker’s microhardness values were measured for the grown crystal. Relative powder second harmonic generation efficiency tested by high intensity Nd: YAG laser as a source is about 60 times greater than that of potassium dihydrogen phosphate.