## Abstract Solid‐state CP/MAS ^31^P NMR spectra were measured for the following unsaturated phosphorus–nitrogen–sulfur ring systems: 1,5‐R~4~P~2~N~4~S~2~ (R = Me, Et, Ph), 1,5‐Ph~4~P~2~N~4~S~2~Ph~2~, Ph~2~PN~4~S~3~NPPh~3~ and Ph~2~PN~3~S~2~. The isotropic solid‐state shifts correlate well with the
Phosphorus-31 NMR studies of stabilized phosphorus ylids in the solid state
✍ Scribed by Glenn H. Penner; William P. Power; Ronald D. Curtis; Roderick E. Wasylishen
- Publisher
- Elsevier Science
- Year
- 1992
- Tongue
- English
- Weight
- 572 KB
- Volume
- 1
- Category
- Article
- ISSN
- 0926-2040
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✦ Synopsis
Phosphorus-31 powder NMR spectra and high-resolution MAS spectra have been obtained for a number of stabilized phosphorus ylids under conditions of high-power proton decoupling and cross-polarization. The 31P CP/MAS spectra are compared to those obtained from isotropic solutions. The variation of chemical shift anisotropy and of the principal components of the 31P chemical shift tensor determined from 31P powder NMR line shapes are discussed in terms of the relative importance of accepted valence bond resonance structures. The results indicate that the invariance of the isotropic chemical shift, delta iso, observed in previous 31P NMR investigations of phosphorus ylids in solution is due to fortuitous cancellation of opposing changes in the principal components, delta 11 and delta 33, of the 31P chemical shift tensor. The 31P dipolar NMR powder spectrum of a typical stabilized ylid, (C6H5)3(31)P-13CHC(O)OCH2CH3, is analyzed in order to obtain the orientation of the 31P chemical shift tensor with respect to the 31P-13C alpha dipolar vector.
📜 SIMILAR VOLUMES
Pure samples and as-prepared mixtures of Rh9 and Rh10 carbonyl clusters with interstitial P atoms have been studied quantitatively by 31P MAS and 1H-31P CP/MAS NMR. Information on the 31P chemical shift tensor of the Rh9 and Rh10 clusters has been derived from spinning sideband simulations. The chem