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SOLID-STATE P-31 NMR INVESTIGATIONS OF UNSATURATED PHOSPHORUS NITROGEN SULFUR RINGS

TitleSOLID-STATE P-31 NMR INVESTIGATIONS OF UNSATURATED PHOSPHORUS NITROGEN SULFUR RINGS
Publication TypeJournal Article
Year of Publication1992
AuthorsChivers, T, Edwards, M, Fyfe, CA, Randall, LH
JournalMagnetic Resonance in Chemistry
Volume30
Pagination1220-1223
Date PublishedDec
Type of ArticleArticle
ISBN Number0749-1581
Keywords1, 5-DIPHOSPHADITHIATETRAZOCINES, BOND, CRYSTAL, ELECTRONIC-STRUCTURES, MAGIC ANGLE, PHOSPHORUS NITROGEN SULFUR RINGS, SOLID-STATE P-31 NMR, SPECTROSCOPY
Abstract

Solid-state CP/MAS P-31 NMR spectra were measured for the following unsaturated phosphorus-nitrogen-sulfur ring systems: 1,5-R4P2N4S2 (R = Me, Et, Ph), 1,5-Ph4P2N4S2Ph2, Ph2PN4S3NPPH3 and Ph2PN3S2. The isotropic solid-state shifts correlate well with the corresponding shifts in solution, the largest difference being 9.0 ppm, indicating that there are no phase-dependent structural features. Analysis of the principal elements of the shielding tensor by the spinning side band method showed that one of these elements is primarily responsible for the anomalously low-field isotropic chemical shifts of 1,5-R4P2N4S2, but no correlation was found between this individual tensor component and any of the structural parameters of these folded eight-membered rings. Two isotropic shifts were observed for the crystallographically inequivalent phosphorus atoms of 1,5-Et4P2N4S2, but the individual P-31 isotropic shifts of 1,5-Me4P2N4S2 were not resolved.

URL<Go to ISI>://A1992KA99300010