| In this paper, four novel Keggin molybdenum phosphates, [Cu(2,2'-bipy)2][PMo8VIMo4VO40 {Cu(2,2'-bipy)}2.5]·H2O 1 {PMo11VIMoVO40[Cu (phen)2]2} 2{PMo11VIMoVO40[Cu (2, 2'-bipy)2]2}·3H2O 3, [Cu2(phen)2Cl][PMo12O40]·0.5H2O 4 (2,2'-bipy=2,2'-bipyridine, phen=1,10-phenanthroline), have been hydrothermally synthesized andcharacterized by IR, XPS, TGA and single-crystal X-ray diffraction. Furthermore, theelectrochemical property of compound 2 was studied via the method of bulk-modified carbonpaste electrodes. In the structure of compound 1, the reduced α-Keggin polyoxoanion[PMo8VIMo4VO40] 7-is capped by two divalent Cu atoms through four bridging oxo groups ontwo opposite {Mo4O4} faces or pits and supports a half {Cu(2,2'-bipy)} complex via thesurface bridging oxygen atoms. Compound 2 and 3 are both disupported-heteropolyoxoanions;unusually, compound 2 shows that two {Cu(phen)2} fragments are supported by the reducedα-Keggin polyoxoanion [PMo11VIMoVO40]4- through a terminal oxygen atom and a bridgingoxygen atom from the opposite sides of the Keggin structure. Compound 4 successfullycombines inorganic-organic copper halide [Cu2(phen)2Cl]3+ cation with a Kegginpolyoxoanion through hydrogen bonds and π-π interactions to obtain a new type of 3Dsupramolecular composite solid-state material.
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