Abstract: A new inorganic-organic hybrid compound [NO2BzPy][Cd(SCN)3], where [NO2BzPy]+ = 1-(4' -nitro-benzyl)pyridinium, was synthesized and characterized by elemental analysis, IR spectroscopy, TG analysis and single-crystal X-ray diffraction. The results of IR analysis show that the SCN- anions are coordinated in a di-1,3-μ bridge mode. Adjacent Cd(II) atoms are linked by three 1,3-μ-SCN- anions forming infinite [Cd(SCN)-3]∞ zigzag polymeric chains. In the crystal structure of the title compound, cations and ations form completely segregated stacking column along the direction of c-axis. Crystal data: monoclinic, space group P2(1)/c with a = 1.1260(3) nm, b = 1.5080(4) nm, c =1.1070(3) nm, β= 105.410(10) °, V = 1.8121(8) nm3, Z = 4, dc = 1.840 g·cm3, T= 293(2) K, μ= 1.571 mm-1, F(000) = 992, R1 = 0.0343, wR2 = 0.0750 [I>2σ(I)].Thermogravimentric analysis reveal the organic molecule is lost in the range of 180-305 ℃ and three SCN- anions are lost after 305 ℃ accompanying the sublimation of cadmium.