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Single crystals of pure, Mg 2? and Sr 2? added Ammonium Tetra Fluoro Antimonates (ATFA) have been grown by slow evaporation technique and reported for the first time. Single crystal X-ray diffraction confirms the grown crystals are monoclinic in structure and the addition of impurities makes the small variation in the lattice parameter. The vibrational frequencies of various group ligands in the crystals have been derived from the Fourier Transform Infrared spectrum. Energy Dispersive Spectroscopy shows the quantitative analysis as well as the confirmation of the inclusion of impurities into the pure ATFA crystal lattice. The optical behaviour and band gap energy are examined by UV-Vis studies. The hardness of the crystal and its thermal stability are studied using microhardness and Thermogravimetric and Differential Thermal Analyzes studies. The addition of impurities increases the thermal stability of the grown crystals which may be one of the added advantages for the electro-optic device fabrication. The dielectric and the electrical behaviour of the grown crystals are also studied and reported.The activation energy of pure, Ca 2? and Sr 2? added ATFA crystals are calculated and it is found to be 0.0608, 0.0596 and 0.0898 eV.

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