| Summary: | A new compound, namely, [Zn(L)<sub>2</sub>]<sub>n</sub> (<b>1</b>) was obtained by the reaction of 2-methyl-4-(4<i>H</i>-1,2,4-triazol-4-yl) benzoic acid (HL) with ZnSO<sub>4</sub>·7H<sub>2</sub>O, and the compound was characterized by single-crystal X-ray diffraction, infrared spectroscopy, elemental analysis, powder X-ray diffraction (PXRD), and thermogravimetric analysis. The linear HL ligands were deprotonated to be L<sup>−</sup> anions and act as two-connectors to link Zn<sup>2+</sup> to form a two-dimensional (2D) lay structure with (4, 4) topology. The large vacancy of 2D framework allows another layer structure to interpenetrate, resulting in the formation of 2D + 2D → 2D parallel interpenetration in <b>1</b>. The weak interactions, such as hydrogen bonding and π⁻π stacking interactions, connect the adjacent 2D layers into a three-dimensional (3D) coordination polymer. The solid-state UV-visible spectroscopy and luminescent property have also been studied.
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