Abstract: Several alkyl-, aryl-, and perfluoroalkylcyclopolyphosphines have been examined by NMR, ir-Raman, and mass spectroscopy. It is found that three-, four-, and five-membered rings can be distinguished in solution by observing the 3'P NMR spectrum while decoupling all other nuclear spins. The decoupled 31P NMR spectrum of a four-membered ring collapses to a sharp singlet, while spectra of the three-and five-membered rings yield ...