: Good quality single crystals of nonlinear optical material Ammonium hydrogen oxalate hemihydrate which crystallizes in Orthorhombic crystal system and belonging to space group Pnma were successfully grown from an aqueous solution by slow evaporation method. The grown crystals were characterised by single crystal X-ray diffraction, Thermal studies, Vickers microhardness test, dielectric studies and photoconductivity study. The Nonlinear optical (NLO) property of the crystal was confirmed by the Kurtz-Perry powder second harmonic generation test.