Abstract: Ammonium Di-hydrogen Phosphate (ADP), crystals are good Second Harmonic Generators (SHG) having appreciable Non Linear Optic (NLO) properties. These ADP crystals when mixed with metallic radicals show a visible modification in the change of growth habit during growth. Bimetallic crystal Nikel Magnesium (Ni3+, Mg2+) Ammonium Di-hydrogen Phosphate (NMADP), when analysed for structural and optical characteristics show a visible change in their properties, compared to the pure crystal of ADP. FTIR investigations reveal that the inclusion of the metallic impurities extend the transmission region to a great extent, where the HRXRD reveals that the crystallinity of the material is superior in the pure form than the bimetallic form conforming the inclusion of the bimetals. The conversion efficiency and SHG generation of the grown crystals were also confirmed.