1H and 13C NMR spectroscopy of four compounds of the type [SbR3X] 2O, where X= Br and R= Ph, p-tolyl and o-tolyl or X= Cl and R= Me, have been interpreted as showing that unless stringent precautions are taken to exclude moisture there is cleavage of the oxygen bridge to give solutions which contain both the hydroxo species, SbR3 (OH) X, and the original bridged compound. This is in agreement with earlier results from IR spectra of compounds ...