The complex {［Zn(BTC)2/3］·［HCON(CH3)2］·［C2H5OH］}n(1) was prepared from 1,3,5-benzenetricarboxylic acid (H3 BTC) and Zn(Ⅱ) cation via a solvothermal technique. The complex 1 was characterized by single crystal X-ray diffraction(SXRD), Fourier transform-infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), powder X-ray diffraction (PXRD) and fluorescence spectroscopy. Single crystal X-ray diffraction analysis indicates that complex 1 belongs to space group P21/n of the monoclinic system. In complex 1, the Zn(Ⅱ) ion is coordinated with BTC3- anion through the oxygen atom on the carboxyl group, forming a three-dimensional Zn(Ⅱ) metal-organic framework (MOF) structure with channels. And through intermolecular hydrogen bond interaction, ethanol and N, N′-dimethylformamide (DMF) molecules are encapsulated into parallelogram channels. Fluorescence spectrum analysis at room temperature shows that when the excitation wavelength is 297 nm, complex 1 has the strongest emission peak at 601 nm.