Coordination polymers of 2′,3′,5′,6′-tetramethyl-1,1′:4′,1′′-terphenyl-4,4′′-dicarboxylic acid with Cu(II), Co(II) and Cd(II) have been synthesized and characterized by IR spectroscopy, single crystal X-ray diffraction, thermogravimetric analysis and nitrogen sorption studies. Display omitted Three new 3D-metal–organic frameworks based on 2′,3′,5′,6′-tetramethyl-1,1′:4′,1′′-terphenyl-4,4′′-dicarboxylic acid (H2L) and Co, Cu, and Cd nodes have been synthesized. The complexes were characterized by elemental, thermogravimetric analysis, IR spectroscopy, single crystal, powder X-ray diffraction and gas sorption experiments. The crystal structure of Cu2L2(H2O)2n (1) corresponds to a two-dimensional coordination polymer, in which the metal nodes are two crystallographically equivalent Cu(II) atoms linked by four μ2-O,O′ carboxylate ligands in a centrosymmetric {Cu2O10} paddle-wheel building block. The structure of compound CoL(dmso)n (2) has a 3D metal–organic coordination lattice, in which the metal centers are connected by the linear organic ligand to generate a dense three-dimensional coordination polymer. Also, a three-dimensional coordination network was identified in the case of compound Cd2L2(dmf)n (3), whose structure is very similar to that of compound 2. In compound 3, the carboxylate groups of the linear L2− spacers behave as μ2-κ3O, O′:O tridentate bridging ligands. The compounds have a high thermal stability. Polymers 3 and 1 have moderate porosity (specific surface areas of approximately 900 m2/g and 600 m2/g, respectively), while polymer 2 has a dense structure.