A three‐dimensional Zn II coordination framework: poly[[μ 2 ‐( E )‐1,2‐bis(pyridin‐4‐yl)ethene][μ 4 ‐( E )‐2,2′‐(diazene‐1,2‐diyl)dibenzoato][μ 2 ‐( E )‐2,2′‐(diazene‐1,2‐diyl)dibenzoato]dizinc(II)]

In the title coordination polymer, [Zn 2 (C 14 H 8 N 2 O 4 ) 2 (C 12 H 10 N 2 )] n , the asymmetric unit contains one Zn II cation, two halves of 2,2′‐(diazene‐1,2‐diyl)dibenzoate anions (denoted L 2− ) and half of a 1,2‐bis(pyridin‐4‐yl)ethene ligand (denoted bpe). The three ligands lie across crystallographic inversion centres. Each Zn II centre is four‐coordinated by three O atoms of bridging carboxylate groups from three L 2− ligands and by one N atom from a bpe ligand, forming a tetrahedral coordination geometry. Two Zn II atoms are bridged by two carboxylate groups of L 2− ligands, generating a [Zn 2 (CO 2 ) 2 ] ring. Each loop serves as a fourfold node, which links its four equivalent nodes via the sharing of four L 2− ligands to form a two‐dimensional [Zn 2 L 4 ] n net. These nets are separated by bpe ligands acting as spacers, producing a three‐dimensional framework with a 4 6 6 4 topology. Powder X‐ray diffraction and solid‐state photoluminescence were also measured.