A one-dimensional coordination polymer, namely catena-poly[[aquapyridinecadmium(II)]-μ(3)-{4,4'-[(2,4,6-trimethyl-1,3-phenylene)bis(methylene)]dibenzoato}], [Cd(C(25)H(22)O(4))(C(5)H(5)N)(H(2)O)](n), has been synthesized by a biphasic solvothermal reaction. The Cd(II) cation is located in a CdO(5)N six-coordinated environment. The trans 4,4'-[(2,4,6-trimethyl-1,3-phenylene)bis(methylene)]dibenzoate ligand connects the Cd(II) cations to form a one-dimensional ribbon incorporating centrosymmetric [Cd(2)(COO)(2)] secondary building units. Inter-ribbon O-H...O hydrogen bonds extend the one-dimensional ribbons into a two-dimensional sheet. No π-π interactions are observed. Comparing products synthesized using a different method, it was found that biphasic solvothermal conditions play a crucial role in obtaining large well-shaped single crystals; only intractable precipitates were obtained by the traditional single-phase solvothermal method.