Abstract: | A novel two‐dimensional (2D) ZnII coordination framework, polyμ‐1,3‐bis(2‐methyl‐1H‐imidazol‐1‐yl)benzene](μ‐5‐nitrobenzene‐1,3‐dicarboxylato)zinc(II)], Zn(C8H3NO6)(C14H14N4)]n or Zn(NO2‐BDC)(1,3‐BMIB)]n 1,3‐BMIB is 1,3‐bis(2‐methyl‐1H‐imidazol‐1‐yl)benzene and NO2‐H2BDC is 5‐nitrobenzene‐1,3‐dicarboxylic acid], has been prepared and characterized by IR, elemental analysis, thermal analysis and single‐crystal X‐ray diffraction. Single‐crystal X‐ray diffraction analysis revealed that the compound is a new 2D polymer with a 63 topology parallel to the (10) crystal planes based on left‐handed helices, right‐handed helical NO2‐BDC–Zn chains and Zn2(1,3‐BMIB)2]n clusters. In the crystal, adjacent layers are further connected by C—H…O hydrogen bonds, C—H…π interactions, C—O…π interactions and N—O…π interactions to form a three‐dimensional structure in the solid state. In addition, the compound exhibits strong fluorescence emissions in the solid state at room temperature. |