<div><p>Two new compounds, [CuCl(Phen)(H<sub>2</sub>O)][PW<sub>12</sub>O<sub>40</sub>][4,4′-H<sub>2</sub>bpy]·1.5H<sub>2</sub>O (<b>1</b>) and [Cd<sub>2</sub>(Phen)<sub>4</sub>Cl<sub>2</sub>][HPMo<sub>12</sub>O<sub>40</sub>](4,4′-bpy) (<b>2</b>) (bpy = bipyridine, Phen = phenanthroline), have been hydrothermally prepared and characterized by IR, UV–vis, XPS, XRD, elemental analysis, cyclic voltammetry analysis, and single-crystal X-ray diffraction analysis. Compound <b>1</b> exhibits a 1-D chain structure constructed from polyoxometalates (POMs) and transition metal complexes, whereas <b>2</b> presents a supramolecular structure constructed from POMs, metal halide clusters, and organic ligands.</p></div
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