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Novel semi-organic single crystals of bis (Lproline) cadmium iodide (BLPC) were grown by slow evaporation technique. The crystal structure was determined by single-crystal X-ray diffraction studies. Singlecrystal X-ray diffraction study shows that [BLPC] crystallizes in orthorhombic system with space group P2 1 2 1 2 1 . 1 H NMR and 13 C NMR studies were conducted for the grown crystal. Functional groups present in the compound were identified by FTIR spectral studies. The UV-Vis-NIR spectrum was studied to analyse the optical properties of the grown crystals. Thermogravimetric analysis was carried out to study thermal behaviour of the materials. Vickers microhardness measurement was carried out for different loads. Etching studies were carried out using water as etchant. The second harmonic generation efficiency was determined by the Kurtz powder method and it was found to be higher than that of potassium dihydrogen phosphate.