Three new coordination compounds, {[Zn(btrp)(ip)]∙2H 2 O} n (1), {[Zn(btrp)(hip)]∙2H 2 O} n (2), and {[Zn 1.5 (btrp)(btc)(H 2 O)]∙H 2 O} n (3) (btrp=1,3-bis(1,2,4-triazol-1-yl)propane, H 2 ip=isophthalate, H 2 hip=5-hydroxy isophthalate, H 3 btc=benzene-1,3,5-tricarboxylic acid) have been prepared via solvothermal method and characterized by single crystal X-ray diffraction and elemental analysis. 1 possesses 2D (4. 4) net framewok. 2 is also a 2D infinite layer framework, and the resulting 2D structure is interconnected by hydrogen-bond and π…π interactions to lead to a 3D supramolecular architecture. 3 exhibits a novel 2D framework with three nonequivalent points, {5.6 2 }{5 2 .6}{5 4 .8 2 }. The fluorescence properties of 1–3 have been studied at room temperature.