The semiorganic non-linear optical crystal bisthiourea magnesium sulphate (BTMS) was grown by slow evaporation technique using water as solvent. Vibrational spectra were recorded to determine the symmetries of molecular vibrations. The observed Raman and infrared bands were also assigned and discussed. The optical transmission spectral study was carried out to test the transmitting ability of the crystal in the visible range. The second harmonic generation test of BTMS revealed the non-linear nature of the crystal. The TGA/DTA curve was also recorded for the experimental crystal.