A new Sb (III) halide complex, [C10H10N2]2 (SbCl4)2 & sdot;2Cl has been successfully created through slow evaporation at room temperature and carefully analyzed using physicochemical methods. This compound which was examined by single-crystal X-ray diffraction, was found to crystallize in the monoclinic system, space group P21/ c with crystallographic parameters a= 14.1119 (8)angstrom, b= 14.2464 (8)angstrom, c= 16.140 (1)angstrom, beta= 109.376 (1) , V= 3061.1 (3)angstrom 3 and Z=4. The cristal lattice was composed of two distorted tetrahedron anions (SbCl4)- and two free chloride anions which are surrounded by two independent 2,2 '-bipyridinium [C10H10N2]2+ cations. This later helps to balance the negative charge of the inorganic part. The way that crystal was arranged, is due to the presence of N-H...Cl hydrogen bonds give rise to a supramolecular structure with three-dimensional network. The vibrational absorption bands were identified by Infrared and Raman spectroscopy which confirm the exis-tence of the organic cations [C10H10N2]2+ and the inorganic part [SbCl4] -2Cl-. The Hirshfeld surface analysis and fingerprint plots methods were employed to identify the different intermolecular interactions in the crystal network and to determine their contribution in the crystal structure construction. The compound provides a good thermal stability up to 117 degrees C studied by thermogravimetric analyses. Furthermore, optical studies confirmed semiconducting properties with the detection of band gap at 3.5 eV. The compound was also exhibited photo-luminescence properties.