Two new zinc(II)–triazole–aliphatic dicarboxylate coordination polymers, [Zn(trz)(Hsuc)] n (1), [Zn 2 (trz) 2 (tar)] n (2), have been hydrothermally synthesized by reaction of Zn salt, Htrz with H 2 suc and H 2 tar, respectively (Htrz=1,2,4-triazole, H 2 suc=succinic acid, H 2 tar=tartaric acid).Their structures were determined by single-crystal X-ray diffraction analyses and further characterized by X-ray powder diffraction, elemental analyses, IR spectra and TG analyses. Compound 1 displays a 2D layer structure containing {[Zn 4 (trz) 4 ] 4+ } n layers decorated by the suc ligand. Compound 2 is in a 3D structure formed by the interconnection of 2D {[Zn 4 (trz) 4 ] 4+ } n layers with tar ligand, resulting a 3,4-connected topological network. Due to the different coordination mode and conformation of aliphatic carboxylate ligand, the similar 2D {[Zn 4 (trz) 4 ] 4+ } n layers stack in the –AAA– fashion in 1, while the {[Zn 4 (trz) 4 ] 4+ } n layers hold together in the –ABAB– stacking sequence in 2. Additionally, the two compounds show strong fluorescence in the solid state at room temperature.