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31 P and 77 Se CP/MAS and 31 P CPECHO solid‐state NMR studies of bis(dineopentoxy‐thiophosphoryl) diselenide and disulphide
Author(s) -
Potrzebowski Marek J.
Publication year - 1995
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.1260330104
Subject(s) - chemistry , diselenide , anisotropy , pulse sequence , selenium , proton nmr , nmr spectra database , crystallography , analytical chemistry (journal) , spectral line , stereochemistry , nuclear magnetic resonance , organic chemistry , optics , physics , astronomy
The principal elements δ ii of 31 P and 77 Se chemical shift tensors for the structural analogues bis(dineopentoxythiophosphoryl) diselenide (1) and bis(dineopentoxythiophosphoryl) disulphide (2) were calculated from spinning sideband intensities employing the MASNMR program. From analysis of the 31 P NMR data it was concluded that replacement of sulphur by selenium has little influence on shielding parameters, anisotropy Δδ and span Ω. The asymmetry η and skew k are very similar if the geometry of SPXXPS unit (X = S, Se) is not changed. 77 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 2d are 0.387 kHz 2 for diselenide 1 and 0.495 kHz 2 for disulphide 2. These values are consistent with those calculated from the van Vleck equation for polycrystalline materials.