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　[Zn2(BYPM)(NPTA)2]n　(1)　has　been　synthesized　under　solvothermal　condition.　The　1　is　characterized　by　elemental　analysis,　Thermogravimetric　analysis　(TGA),　single-crystal　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　Zn2+　ions　and　further　forms　a　three-dimensional　supramolecular　framework　through　intermolecular　C−H⋅⋅⋅O　and　C−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.　©　2022　Wiley-VCH　GmbH.