The semi-organic lithium hydrogen phthalate dihydrate (LHP dihydrate) was synthesized. The LHP dihydrate single crystal was grown by slow evaporation solution technique with water as solvent. Transparent, colourless crystal of size 10 mm x 10 mm x 50 mm with well-defined morphology was grown. The grown crystals were characterized by powder and single-crystal X-ray diffraction, FT-IR. UV-vis, fluorescence, dielectric, TG/DTA and micro hardness studies. The crystal structure and the unit cell parameters were analyzed from the X-ray diffraction studies. The structural perfection of the grown crystal has been analyzed by high-resolution X-ray diffraction (HRXRD) rocking curve measurements. The FT-IR spectrum analysis has confirmed the functional group in the LHP dihydrate single crystals. The range and percentage of optical transmission are ascertained by recording the UV-vis spectrum. The thermal behavior of the crystals has been investigated by TG/DTA analysis. (C) 2009 Elsevier B.V. All rights reserved.