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The 1H NMR spectrum of, n-C4H9 4N]3[IMo6O22(OMe)2] gives two peaks assignable to the methyl groups of the anion in roughly a 2:1 ratio, although they are equivalent in the solid state. Partial hydrolysis of the [IMo6O22(OMe)2]3- anion to form the monomethylated [IMo6O23(OMe)]4- anion is one possible explanation but has been excluded because the monomethylated anion gives a single peak with a chemical shift different from both of those peaks. The intensity ratio of those peaks does not change with the concentration of the compound or the amount of methanol in solution either. Hindered rotation of the methyl groups is another possible explanation but has also been rejected because they give two peaks in roughly a 2:1 ratio even in the 13C NMR spectra. We currently have no solid explanation for this observation
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