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[Me4N]+[SO2F3]−, the first example of a [SO2F3]− salt, has been prepared from Me4NF and SO2F2. The colorless, microcrystalline solid was characterized by its infrared and Raman spectra. The trigonal bipyramidal structure of C2v symmetry of the [SO2F3]− anion is predicted by ab initio calculations. Two oxygen atoms with d(SO)=143.2 pm and one fluorine atom with d(SF)=157.9 pm occupy the equatorial...
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