The potentiometric titrn. of a ﾎｳ-Keggin tetra-protonated silicodecatungstate, [ﾎｳ-SiW10O34(H2O)2]4- (H4ﾂｷI), with TBAOH (TBA = [Bu4N]+) showed inflection points at 2 and 3 equiv of TBAOH. The 1H, 29Si, and 183W NMR data suggested that the in situ formation of tri-, doubly-, and monoprotonated silicodecatungstates, [ﾎｳ-SiW10O34(OH)(OH2)]5- (H3ﾂｷI), [ﾎｳ-SiW10O34(OH)2]6- (H2ﾂｷI), and [ﾎｳ-SiW10O35(OH)]7- (HﾂｷI), with C1, C2v, and C2 symmetries, resp. Single crystals of TBA6ﾂｷH2ﾂｷI suitable for the x-ray structure anal. were successfully obtained and the anion part was a monomeric ﾎｳ-Keggin divacant silicodecatungstate with two protonated bridging O atoms. Compds. H3ﾂｷI, H2ﾂｷI, and HﾂｷI were reversibly monoprotonated to form H4ﾂｷI, H3ﾂｷI, and H2ﾂｷI, resp. [on SciFinder(R)]
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