Abstract A novel three-dimensional coordination compound has been solvothermally synthesized based on a tetracarboxylate ligand H4L (H4L = 1,3,6,8-tetrakis(4-carboxylphenyl)pyrene), Zn2L(H2O)2·2DEF (1) (DEF = N,N′-diethylformamide). Each Zn ion is coordinated by four carboxylate oxygen atoms from four L4− ligands and one oxygen atom from a water molecule to provide a distorted square-pyramidal geometry. Pairs of adjacent Zn cations are bridged by four carboxylate groups of four different L4− ligands to generate a paddle-wheel [Zn2(COO)4(H2O)2] secondary building unit (SBU). Each SUB is further linked to four L4− ligands to give a three-dimensional framework with cds-type (CdSO4-type) topology. The crystal structure has been determined via single-crystal X-ray diffraction, and the compound was characterized by elemental and thermal analysis, infrared spectroscopy, powder X-ray diffraction, and solid-state photoluminescence measurements.