## Abstract The principal elements of the chemical shift tensors for the phosphorus atoms in three bis(dialkoxythiophosphoryl) disulfides were determined from both static and magic angle spinning NMR spectra, using the intensities of the peaks in the spinning sidebands relative to those of the cent
X-Ray and 31P CP MAS NMR studies of bis(dialkoxythiophosphoryl) disulfides
β Scribed by Marek J. Potrzebowski; Joseph H. Reinbenspies; Zhiang Zhong
- Publisher
- John Wiley and Sons
- Year
- 1991
- Tongue
- English
- Weight
- 451 KB
- Volume
- 2
- Category
- Article
- ISSN
- 1042-7163
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β¦ Synopsis
The crystal and molecular structures of the title compounds were determined by X-ray diffraction technique from diffractometer intensity measurements. It has been found that two homologous disulfides, bis(dimethoxythiophosphory0 disulfide 1 and bis(dineopentoxythiophosphory0 disulfide 2, form different molecular and crystal structures with space groups C2Ic and P?, respectively. These results were confirmed by 3'P CP MAS NMR studies, which showed that under favorable conditions the solid state N M R may lead to determination of the number of crystallographically unique phosphovus atoms. Moreover, the variation of the disulfide S-S bond length versus torsional P-s-S-P angles was observed.
π SIMILAR VOLUMES
## The principal elements Sii of 31P and '"Se chemical shift tensors for the structural analogues bis(dineopentoxythiophosphory1) diselenide (1) and bis(dineopentoxythiophosphory1) disulphide (2) were calculated from spinning sideband intensities employing the MASNMR program. From analysis of the
The reactions between triphenylphosphine sulfide (Ph 3 PS) and ICl in CCl 4 and IBr in CH 2 Cl 2 in 1 : 1 molar ratio give the solid adducts Ph 3 PS Β΄ICl (I) and Ph 3 PS Β΄IBr (II) whose structures have been solved by X-ray diffraction. Compounds I and II consist of discrete molecule units and featur