High-energy photoelectron (p.e.) spectra have been obtained for a number of compounds of antimony. The antimony 3d(,5//2) binding energies range from 542.9, 533.3 eV for [Et4N][SbF6] to 538.6, 529.0 eV for Bun3Sb, but there is little correlation with the formal oxidation state. Assignment of the oxidation state of antimony on the basis of X-ray p.e. data alone is not possible with certainty and even gross structural differences may remain undetected by this method.
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Birchall et al. (1975) studied this question.
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