A terpyridine/Zn-based metal–organic framework (MOF) with the formula [Zn2(terpyb)2(amtp)]n was prepared starting from 4-(4,2′:6′,4″-terpyridin-4′-yl)benzoic acid (terpyb) and aminoterephthalic acid (amtp) ligands and Zn(II) metal ions. Single-crystal X-ray crystallography confirmed the formation of a 3D triply interpenetrated structure containing distorted tetrahedral Zn(II) ions, each coordinated to one carboxylate oxygen and two N donor atoms from three symmetry-related terpyb ligands along with a carboxylate oxygen of the amtp anion. In turn, the terpyb ligands each bond to three metal atoms, while the amtp ligands bridge pairs of metal atoms. The structure of the MOF was also analyzed using powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), Raman spectroscopy, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). The MOF exhibited high catalytic …