Biphase synthesis of a one‐dimensional coordination polymer based on a dinuclear CdII secondary building unit and a novel semi‐rigid dicarboxylate

A one‐dimensional coordination polymer, namely catena‐polyaquapyridinecadmium(II)]‐μ₃‐{4,4′‐(2,4,6‐trimethyl‐1,3‐phenylene)bis(methylene)]dibenzoato}], Cd(C₂₅H₂₂O₄)(C₅H₅N)(H₂O)]_n, has been synthesized by a biphasic solvothermal reaction. The Cd^II cation is located in a CdO₅N 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 Cd₂(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.