187Os, 31P and 17O NMR study of carbonylated and alkylated (p-cymene)OsI (L)PR3 complexes

Autor: Eric J. M. Meier, Martina Schaade, Andreas Gisler, Anthony Linden, Wolfgang von Philipsborn
Rok vydání: 1997
Předmět:
Zdroj: Journal of Organometallic Chemistry. :315-326
ISSN: 0022-328X
Popis: Series of complexes of the types [(p-cymene)OsI(CO)PR3][PF6], (p-cymene)OsI(phenylethynyl)PR3, (p-cymene)OsI(alkyl)PR3 have been prepared and investigated by 187Os, 31P and 17O NMR spectroscopy. The structures of (p-cymene)OsI(C=CPh)PMe3 (3a) and (p-cymene)OsI(C=CPh)PiPr3 (3c) have been determined by X-ray diffraction. A mechanistic study of the formation of the metallacycle 8A formed by intramolecular trans-alkylation from (p-cymene)0sI2PiPr3 (1c) in the presence of Al2Me6 is presented. As shown by time-dependent 31P NMR, (p-cymene)OsI(Me)PiPr3 (6c) is formed as an intermediate. 187Os,13C coupling constants in Cp- and Cp*Os(CO)2Me (14 and 15) have been determined from 13C-filtered (1H, 187Os)-HMQC correlation spectra and are interpreted in comparison with the 57Fe,13C data of the corresponding iron complexes.
Databáze: OpenAIRE