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The new organic-inorganic compound, [(C 6 H 7 N 2 O 2) 3 TeCl 5 .2Cl] was synthesized and its structure was determined at room temperature in the triclinic system (P ̅ 1) with the following parameters: a= 10.5330(11)Å, b= 10.6663(11) Å, c= 15.9751(16)Å, α= 82.090(2)°, β= 71.193(2)°, γ= 68.284(2)° and Z = 2. The final cycle of refinement led to R= 0.057 and R w = 0.149. The crystal structure was stabilized by an extensive network of N-H...Cl and nonclassical C-H…Cl hydrogen bonds between the cation and the anionic group. Several thermal analysis techniques such as thermogravimetric analysis, the differential scanning calorimetric analysis and Evolved Gas Analysis were used. We used isoconversional kinetics methods to determine the kinetics parameters. We observe that the decomposition of [C 6 H 7 N 2 O 2 ] 3 TeCl 5 .2Cl entails the formation hydrochloric acid of nitroaniline as volatiles. The infrared spectra were recorded in the 4000-400 cm-1 frequency region. The Raman spectra were recorded in the external region of the anionic sublattice vibration 50-1500 cm-1. The optical band gap was calculated from the UV-Vis absorbance spectra using classical Tauc relation which was found to be 3.12 and 3.67 eV.