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)₂]_n (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.