In this work, we have successfully introduced the nitrogen-rich aromatic ligand 5,5'-bipyrimidine (BYPM) as auxiliary ligands into the 3-nitrophthalic acid (NPTA) system, and a Zn(II)-based coordination polymer [Zn 2 (BYPM)(NPTA) 2 ] n (1) has been synthesized under solvothermal condition. The 1 is characterized by elemental analysis, Thermogravimetric analysis (TGA), singlecrystal X-ray diffraction, and X-ray diffraction patterns (PXRD). The single-crystal X-ray analysis indicates that 1 propagates into a layer-like framework along the ac plane through the coordination Zn 2 + ions and further forms a three-dimensional supramolecular framework through intermolecular CÀ H•••O and CÀ H•••N hydrogen bonds. Thermogravimetric analysis and powder X-ray diffraction experiments indicate that 1 has high thermal and solvent stability. Meanwhile, the fluorescence of 1 has been explored.