Abstract: | Two coordination polymers, Co(phen)(oba)(H2O)2] ( 1 ) and Cd3(phen)3(oba)2(Hoba)2(H2O)2] ( 2 ) (oba = 4, 4′‐oxybis(benzoate), phen = 1, 10‐phenanthroline) have been synthesized under hydrothermal conditions. Complex 1 crystallizes in monoclinic, P21/n, a = 7.543(6), b = 33.05(2), c = 9.902(5)Å, β = 103.69(2)°, V = 2398(3)Å3, Z = 4; 2 in monoclinic, P2/n, a = 15.11(1), b = 10.069(8), c = 28.02(2)Å, β = 101.83(1)°, V = 4174(5)Å3, Z = 2. X‐ray single‐crystal diffraction investigations shows that the complexes 1 and 2 consist of helical chains, which are further assembled into layers and networks via supramolecular interactions such as π—π stacking interactions and hydrogen bonds, respectively. The results indicate that the coordination environment is one of the most important factors for assembly of single‐stranded helical chains into double‐stranded helical chains via supramolecular interactions. |