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Semiorganic nonlinear optical single crystals of Bisthiourea potassium sulphato Oxalate (BTKSO) are successfully grown by slow solvent evaporation technique at ambient temperature. The structural property of grown BTKSO crystal was determined by single crystal X-Ray diffractometer. It reveals the triclinic structure with the space group of P1, and the lattice parameters are a = 9.4 ± 0.5Ǻ, b = 10.1 ± 0.5Ǻ, c = 15.7 ± 0.8Ǻ, V = 1400 ± 200Ǻ 3 . Fourier transform infrared (FTIR) studies substantiate the functional groups of the present crystal and the presence of elements was confirmed by employing energy dispersive spectroscopic technique. The optical behavior and transparency nature of BTKSO crystal were studied by UV-Vis-NIR spectra. The Kurtz powder technique is used to ascertain the nonlinear optical behavior of the grown crystal. Its second harmonic conversion efficiency (SHG) is found to be 1.31 times higher than that of reference potassium dihydrogen phosphate (KDP) material. The photoluminescence spectrum of the title crystal shows the strong green emission at 573 nm. The thermal and mechanical behaviors of the grown crystal were studied by thermo gravimetric and differential thermal analyzer (TG/DTA) and Vicker"s hardness test respectively.