IR Spectra, R am an Spectra, Mass Spectra, T riphenyltin D im eth y lp h o sp h in ate T he reactions of (P h 3Sn)20 with P hM eP O C l and w ith P h2P O C l lead to P h 3S n 0 2PM ePh and P h 3S n 0 2PPh2, respectively. Ph3S n 0 2P M e2 has b een p re p a red from the reactio n of (P h 3S n)20 and M e2P 0 2H in toluene. The IR and R am an spectra o f Ph3S n 0 2PM e2, P h 3S nÖ 2PM ePh and P h3S n 0 2P P h2 are found to be consistent w ith polym eric stru ctu res with p entacoordinated tin atom s. The E l mass spectra indicate th a t the principal fragm entation processes of Ph3S n 0 2P R R ' (R R ' = M e2, M ePh, P h2) a p p ear to occur by loss o f phenyl radicals from tin and by elim ination of th e en tire d io rg an o p h o sp h inate group.