A 1D chain-like organic/inorganic composite material with polyoxovanadates serving as building blocks has been synthesized by the reaction of cyclohexylamine with vana- dium pentoxide, and characterized by IR, UV spectra and TG-DTA technique. The title compound (C30H70N5O15V5, Mr = 995.61) crystallizes in orthorhombic, space group P212121 with a = 6.0093(12), b = 26.780(5), c = 27.979(6) ? V = 4502.6(16) 3, Z = 4, Dc = 1.461 g/cm3, F(000) = 2060, = 1.063 mm-1, R = 0.0651 and wR = 0.1084 for 3426 observed reflections (I > 2(I)). Single-crystal X-ray structural analysis indicates that the title compound consists of five proto- nated cyclohexylamine molecules and a polyoxovanadate anion of V5O155-. In addition, the results of IR spectra and single-crystal X-ray diffraction exhibit that there exists comparatively stronger interaction between the organic groups and polyoxovanadate anion in solid state. Adjacent structure units are bridged through corner-sharing oxygen atoms of VO4 tetrahedra to construct a novel one-dimensional zigzag infinite linear chain arrangement. The curves of TG- DTA elucidate that the process of weight loss of the title compound is divided into two stages, and also reveal that the framework of polyoxovanadate anion decomposes at 473.0 ℃. A 1D chain-like organic / inorganic composite material with polyoxovanadates serving as building blocks has been synthesized by the reaction of cyclohexylamine with vana-dium pentoxide, and characterized by IR, UV spectra and TG-DTA technique. The title compound (C30H70N5O15V5, Mr = 995.61) crystallizes in orthorhombic space group P212121 with a = 6.0093 (12), b = 26.780 (5), c = 27.979 (6)? V = 4502.6 (16) 3, Z = 4, Dc = 1.461 g / cm3 R = 0.0651 and wR = 0.1084 for 3426 observed reflections (I> 2 (I)). Single-crystal X-ray structural analysis shows that the title compound consists of five Protonated cyclohexylamine molecules and a polyoxovanadate anion of V5O155-. In addition, the results of IR spectra and single-crystal X-ray diffraction show exhibit that there exists comparatively stronger interaction between the organic groups and polyoxovanadate anion in solid state. Adjacent structure units are bridged through corner-sharing oxygen atoms of VO4 tetrahed ra to construct a novel one-dimensional zigzag infinite linear chain arrangement. The curves of TG-DTA elucidate that the process of weight loss of the title compound divided into two stages, and also reveal the framework of polyoxovanadate anomalies at 473.0 ° C .