The new semiorganic potassium sulphato oxalate (KSO) single crystals are grown at room temperature by a slow evaporation method using an aqueous solution. The Fourier transform infrared spectroscopy is used to ascertain the various functional groups present in the grown KSO sample. The single crystal X-ray diffractometer (XRD) results confirm the grown KSO crystal is a triclinic structure with lattice parameters a = 6.37Å; b = 7.03Å; c = 10.61Å; and space group P1. Powder XRD study proves the crystallinity and purity of the grown crystal. The optical behaviors of KSO are analyzed by UV-vis-near infrared reflectance (NIR) spectrophotometer. Photoluminescence (PL) studies of KSO reveal its strong green emission at 576 nm. The laser damage threshold (LDT) of the title compound is measured to be 6.135 GW/cm 2 . The thermo gravimetric and differential thermal analysis indicated that KSO is stable up to 103°C. From the Vickers microhardness tester, the mechanical behaviors of the title compound are studied. The frequency conversion property of KSO crystal is analyzed using Kurtz-Perry method, and it is found to be 1.16 times higher than that of the reference potassium dihydrogen phosphate which indicates KSO is well suited for optoelectronic device fabrication. KSO was synthesized [13] using potassium sulphate (analar grade) and oxalic acid (analar grade) in a stoichiometric ratio of 1:1.