Unusual formation of a λ 6P-tetrafluorophosphate involving intramolecular donor–acceptor interaction; x-ray crystal structure analysis and temperature-dependent NMR-spectra
✍ Scribed by Thomas Kaukorat; Peter G. Jones; Reinhard Schmutzler
- Publisher
- John Wiley and Sons
- Year
- 1991
- Tongue
- English
- Weight
- 430 KB
- Volume
- 2
- Category
- Article
- ISSN
- 1042-7163
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✦ Synopsis
The N,N,N'-trimethylethylenediaminetetrafluorophosphate, 4, was formed in the unusual reaction of N,N,N'-trimethyl-N'-trimethyl.silylethylenediamine, 1, with the N-P-bonded tetrafluorophosphoranes, dimethylaminotetrafluorophosphorane, 2, or morpholinotetrafluorophosphorane, 3. There was no evidence for the cleavage of a P-F bond in the tetrafluorophosphoranes (with formation of Me3SiF); instead, the Si-N compounds, R2N-SiMe3 (R2 = Me2 or O(CH2CH2)2) were formed. The 19F and 31PNMR spectra o f 4 at room temperature indicated dynamic behavior. The X-ray crystal structure analysis o f 4 resealed the presence of a five-membered ring, formally as a result of iniramolecular donor-acceptor interaction (P-N = 196.5 pm) between the nitrogen atom of the Me2N group and phosphorus.