Two coordination polymers, [Co(µ4-L)(H2 O)2 ]n (1) and [Ni(µ-L)(H2 O)4 ]n (2), were solvothermally assembled from the corresponding metal(II) chlorides and biphenyl-4,4-dioxydiacetic acid (H2 L) as a flexible dicarboxylate linker. The cobalt(II) compound 1 featured a layer-pillared 3D metal-organic network with a cds topology, while the nickel(II) derivative 2 represented a linear chain 1D coordination polymer with a 2C1 topology. The µ4− and µ-L2− linkers exhibited different denticity and coordination modes in the synthesized compounds, thus contributing to their structural diversity. The dimensionality of 1 and 2 had an influence on their thermal stability and decomposition processes, which were investigated in detail by TG-DSC and TG-FTIR methods. Thermal decomposition products of coordination polymers were also analyzed by PXRD, confirming the formation of Co3 O4 /CoO and NiO as final materials. The obtained compounds broaden a family of coordination polymers assembled from flexible dicarboxylate linkers. © 2021 by the authors. Licensee MDPI, Basel, Switzerland.