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The dimeric, sandwich-type tungstophosphate [{PhSbOH}(3)(A-alpha-PW(9)O(34))(2)](9-) (1) has idealized D(3h) symmetry and represents the first organoantimony-containing polyoxometalate. Polyanion 1 was synthesized in an aqueous, acidic medium via three different routes and was fully characterized in the solid state by X-ray diffraction, IR, and thermogravimetric analysis and in solution by multinuclear NMR ((1)H, (13)C, (31)P, and (183)W).

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The formation and crystal structure of [(Cp2Ti)2(SbR2)2] (1, R=Et), [(Cp2Ti)3(SbR)3Sb] [2, R=2-(Me2NCH2)C6H4], and [(Cp2Ti)5(SbR)2Sb7] (3, R=Me3SiCH2) is reported.