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The weak resonances at + 22 and + 49 ppm appearing in the  31 P NMR spectrum of melts or solutions of (PPh) 5  that have been attributed previously in the literature to “dimeric” and “monomeric phenylphosphorus” are caused by (PPh) 6  and (PPh)4, respectively. This was proved by comparison with the  31 P NMR parameters of related compounds and by  31 P NMR spectroscopic investigation of authentic samples of (PPh) 6  and (PPh) 4 , the latter of which was prepared in high yield from (Me 3 Si)PhP–PPh–PPh(SiMe 3 ) and PhPCl 2 . (PEt)4 and mixed-substituted phenyl-ethyl-cyclotetraphosphanes exhibit similar chemical shifts as (PPh)4, corresponding mixed-substituted cyclohexaphosphanes have similar chemical shifts as (PPh) 6 . Generally, cyclophosphanes establish an equilibrium between (PR) n -species of different ring-size. Probably, the ring-interconversion proceeds via a multi-center mechanism. No  31 P NMR spectroscopic evidence for the existence of free PPh or P 2 Ph 2  under the conditions described could be detected. On thermolysis of (PEt)4 the existence of (PEt) 3  was proved for the first time.

zeitschrift für naturforschung b

Beiträge zur Chemie des Phosphors, 62 1  Zur Frage des  31 P-kernresonanzspektroskopischen Nachweises von monomerem und dimerem Phenylphosphor und der Ringgröße von Organyl-cyclophosphanen.: Contributions to the Chemistry of Phosphorus, 62 1  About the Question of  31 P NMR Spectroscopic Detection of Monomeric and Dimeric Phenyl Phosphorus and the Ring Size of Organylcyclophosphanes