The β-alanine doped glycine phosphite (β-alanine-GPI) single crystals were grown from slow evaporation and Sankaranarayanan and Ramasamy (SR) method. The colourless β-alanine-GPI crystal with cylindrical shape about 22 mm diameter and 43 mm length was obtained by this method. The single crystal, powder X-ray diffraction and highresolution X-ray diffraction studies were carried out for β-alanine doped GPI and the results analyzed with pure-GPI. The functional groups and optical properties of β-alanine-GPI were studied by Fourier transform infrared (FTIR) spectroscopy and UV-visible spectroscopy respectively. The results of all these characterizations are discussed in detail.