“…31 P, 13 C, 1 H-NMR spectroscopy allowed for characterization of both diastereomers whereas recrystallization permitted the characterization of (1a,Z) (1,3,2,4-oxathiadiphospholane, 5,5-dimethyl-2,4-diphenyl-2,4-disulfide,(Z)-) by XRD. In addition, mechanistic studies allowed for the elucidation of synthetic intermediates to the heterocyclic intermediates including 1,3,2,4,5-dithiatriphospholane-2,4,5-triphenyl-,2-sulfide (2) ((PhP) 3 S 3 ) and 1,3,2,4-oxathiadiphospholane-5,5-dimethyl-2,4-diphenyl-2-sulfide (3a)/(3b) ((PhP S)(PhP)SOCMe 2 ).…”