A new organic non-linear optical salt 3-nifroaniliniurn trichloroacetate has been synthesized and single crystals grown by slow solvent evaporation solution growth technique at room temperature using methanol as the solvent. The H-1 and C-13 Nuclear magnetic resonance spectra were recorded to establish the molecular structure of the title salt. The crystal structure of the title crystal has been determined by single crystal X-ray diffraction analysis and it belongs to monoclinic crystal system with non-centrosymmetric space group P21. Fourier transform infrared spectral study has been carried out to confirm the presence of various functional groups. The optical transmittance spectrum was recorded in the range 200-2500 nm, to find the optical transmittance window and lower cut off wavelength. The therm gravimetric and differential thermal analyses were carried out to establish the thermal stability of the title crystal. The second harmonic generation in the title crystal was confirmed by the modified Kurtz-Perry powder Lest employing the Nd: YAG laser as the source for infrared radiation. (C) 2013 Elsevier B.V. All rights reserved.