Organoantimony-Containing Polyoxometalate: [{PhSbOH}₃(A-α-PW₉O₃₄)₂]⁹⁻

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).