Two new d 10 metal-organic frameworks based on a novel semi-rigid aromatic biscarboxylate ligand, namely, [Zn (RGAA)(BPY) 1/2 ] (1) and [Cd 5 (μ 3-OH) 2 (RGAA) 4 ] (2) [H 2 RGAA = 4-(carboxymethyl)-2-ethoxybenzoic acid, BPY = 4,4 0-bipyridine], have been synthesized by the hydrothermal reaction, and characterized by Fourier transform-infrared, elemental analyses, X-ray single-crystal diffraction, powder X-ray diffraction and thermogravimetric analyses. Complex 1 displays a three-dimensional (3D) network with a (2,3,4)connected (6ˆ3.8ˆ2.10) 2 (6ˆ3) 2 (8) topology, while complex 2 exhibits a 3D framework with a (3,10)-connected (3.4.5) 2 (3ˆ4.4ˆ6.5ˆ18.6ˆ14.7ˆ2.8) topology. The luminescent properties of compounds 1 and 2 have been investigated in detail, where the emission maxima are 464 and 349 nm, respectively.