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Single crystals of 8-HydroxyQuinoline (8-HQ) and Benzophenone substituted 8-HydroxyQuinoline (B8-HQ) are grown by slow evaporation of acetone at room temperature. Coloured crystals of 8-HQ and B8-HQ with good optical quality of dimensions 54 × 3 × 1.5 mm 3 and 27 × 3 × 1 mm 3 are harvested. Single crystal X-ray diffractometer was utilized to measure the unit cell parameters and to confirm the crystal structure. The presence of various functional groups in the molecule was ascertained by FTIR spectral analysis. The cut off wavelength of 8-HQ and B8-HQ was centered at 350 and 356 nm. The functional groups in the molecule are elucidated by 1 H and 13 C-NMR spectral analyses. Kurtz Perry test confirms the SHG in8-HQ andB8-HQ single crystals.