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In recent years, coordination polymers constructed from multidentate carboxylate ligands and N‐containing ligands have attracted much attention since these ligands can adopt a rich variety of coordination modes which can lead to crystalline products with intriguing structures and interesting properties. A new coordination polymer, namely poly[[diaqua[μ‐2,7‐bis(1H‐imidazol‐1‐yl)fluorene‐κ2N3:N3′][μ‐5,5′‐methylenebis(3‐carboxy‐2,4,6‐trimethylbenzoato)‐κ2O1:O1′]zinc(II)] hemihydrate], {[Zn(C23H22O8)(C19H14N4)(H2O)2]·0.5H2O}n, 1, was prepared by the self‐assembly of Zn(NO3)2·6H2O with 5,5′‐methylenebis(2,4,6‐trimethylisophthalic acid) (H4BTMIPA) and 2,7‐bis(1H‐imidazol‐1‐yl)fluorene (BIF) under solvothermal conditions. The structure of 1 was determined by elemental analysis, single‐crystal X‐ray crystallography, powder X‐ray diffraction, IR spectroscopy and thermogravimetric analysis. Each ZnII ion is six‐coordinated by two O atoms from two H2BTMIPA2− ligands, by two N atoms from two BIF ligands and by two water molecules, forming a distorted octahedral ZnN2O4 coordination geometry. Adjacent ZnII ions are linked by H2BTMIPA2− ligands and BIF ligands, leading to the formation of a two‐dimensional (2D) (4,4)‐sql network, and intermolecular hydrogen‐bonding interactions connect the 2D layer structure into the three‐dimensional (3D) supramolecular structure. Each 2D layer contains two kinds of helices with the same direction, which are opposite in adjacent layers. The luminescence properties of complex 1 in the solid state have also been investigated. A new two‐dimensional coordination polymer based on 5,5′‐methylenebis(2,4,6‐trimethylisophthalic acid) and 2,7‐bis(1H‐imidazol‐1‐yl)fluorene has been prepared and structurally characterized. [ABSTRACT FROM AUTHOR]