Polyoxometalate Derivatives with Multiple Organic Groups. 2. Synthesis and Structures of Tris(organotin) α, β-Keggin Tungstosilicates

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Abstract
Eight tris(organotin)-substituted Keggin tungstosilicate heteropolyanions have been synthesized and characterized by elemental analysis, infrared and Mössbauer spectroscopy, multinuclear NMR, and X-ray crystallography. The new anions contain α- or β-SiW9O3410- moieties and are of two structural types, [(RSn)3(SiW9O37)]7- (R, isomer: Ph, α-, 1; n-Bu, α-, 2; Ph, β-, 3; n-Bu, β-, 4) and [(RSnOH)3(SiW9O34)2]14- (Ph, α-, 5; n-Bu, α-, 6; Ph, β-, 7; n-Bu, β-, 8). Crystals of Cs4H3[(PhSn)3(SiW9O37)]·8H2O (anion 3) are monoclinic, space group C2/c, with lattice constants a = 48.91(2) Å, b = 12.111(3) Å, c = 20.334(9) Å, β = 102.30°, and Z = 8. The anion has nominal C3v symmetry and has a structure with three corner-shared WO6 octahedra of the β-Keggin anion replaced by three PhSnO5 groups. Crystals of Cs9H5[(BuSnOH)3(SiW9O34)2]·36H2O (anion 6) are tetragonal, space group P4̄21m, with lattice constants a = b = 29.005(4) Å, c = 13.412(4) Å, and Z = 4. The anion has the anticipated D3h symmetry and contains three BuSnOH groups sandwiched between A,α-SiW9O3410- anions.

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