Materials crystallizing in noncentrosymmetric (NCS) structures may show certain properties such as pyroelectricitiy, piezoelectricity, ferroelectricity, and nonlinear optical properties. To achieve a macroscopic NCS structure, bismuth, tellurium, and NO₃^- were used in the synthesis as constituents. Since the lone pairs on Bi³⁺ and Te⁴⁺ cations are stereochemically active, they can exhibit asymmetric coordination environment. The π-conjugated electron in the NO₃^- group can also facilitate the nonlinear optical property. The hydrothermally synthesized material reveals a layered nonpolar structure with a weak hydrogen bond interaction. The compound crystallizes in the orthorhombic space group, P2₁2₁2₁. Two types of existing telluriums, Te⁴⁺ and Te⁶⁺ show see-saw and octahedral coordination environment with oxide ligands, respectively. Bi³⁺ cations are linked to oxygen atoms and form BiO₉ and BiO₁₀ polyhedra. NO₃^- is connected to the bismuth atoms. Powder second-harmonic generation (SHG) measurements indicate that the NCS material has a SHG efficiency of 20 times that of α-SiO₂. Further experiments were performed to exfoliate the layers of the material. By adding diluted hydrazine to the sonicated crystals, exfoliated products were obtained, which were characterized by X-ray diffraction and SEM.