The synthesis of a series of cyclic pentaoxyphosphoranes containing a sulfonyl group was carried out by the reaction of either P (OCH2CF3) 3 or P (OPh) 3 with the appropriate diol in an oxidative addition reaction: O2S [(t-Bu) MeC6H2O] 2P (OCH2CF3) 3 (1), O2S [(t-Bu) MeC6H2O] 2P (OPh) 3 (2), O2S [(t-Bu) 2C6H2O] 2P (OCH2CF3) 3 (4), and O2S [(t-Bu) 2C6H2O] 2P (OPh) 3 (5). Reaction of 2 with catechol yielded O2S [(t-Bu) MeC6H2O] 2P ( ...