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31P and 77Se CP/MAS and 31P CPECHO solid-state NMR studies of bis(dineopentoxy-thiophosphoryl) diselenide and disulphide

✍ Scribed by Marek J. Potrzebowski

Publisher: John Wiley and Sons
Year: 1995
Tongue: English
Weight: 606 KB
Volume: 33
Category: Article
ISSN: 0749-1581
DOI: 10.1002/mrc.1260330104

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✦ Synopsis

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 31P NMR data it was concluded that replacement of sulphur by selenium has little influence on shielding parameters, anisotropy A6 and span a. The asymmetry q and skew K are very similar if the geometry of S=PXXP=S unit (X = S, Se) is not changed. "Se NMR data are discussed in terms of PSeSeP unit geometry. The static spectra were recorded employing the CPECHO pulse sequence. It was found that this technique is useful both for the lineshape analysis and the calculation of the second moment. The experimental values of M,, are 0.387 kHz2 for diselenide 1 and 0.495 kHzZ for disulphide 2. These values are consistent with those calculated from the van Vleck equation for polycrystalline materials.

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