LAUSR

Abstract Two new hybrid compounds, [Cu(1)(phen)(H2O)][Cu(2)(phen)(H2O)]([Cu(3)]0.25(H2O)][P2Mo5O23]·3.75H2O (1) and [Cu(en)2]1.5[P2Mo5O23]2·(enH2)3·2H2O (2) (phen = 1,10-phenanthroline, en = ethylenediamine), have been hydrothermally synthesized and characterized by IR, UV–Vis spectroscopy, X-ray photoelectron spectroscopy (XPS), powder XRD analyses, TG analyses, cyclic voltammogram analyses, elemental analyses, and single crystal X-ray diffraction analyses. Single crystal X-ray diffraction analyses reveal that the two compounds have a 1-D chain structure formed by Strandberg-type POMs and TMCs with –A–B–C–B–A–B–C–B– linking mode, then further extend into a 2-D layer structure through π⋯π or hydrogen bond interactions.