C-13 AND P-31 SOLID-STATE NMR-STUDIES OF BIS(DIALKOXYTHIOPHOSPHORYL) DISULFIDES

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 central band in the latter method. These studies show that it is possible to deduce a mode of molecular motion in the solid state by analysis of the shielding parameters. Variable‐temperature 13C and 31P CP MAS NMR of these samples from 190 to 320 K revealed a peculiar motion of the methoxy group and a rigid PSSP backbone for bis(dimethoxythiophosphoryl) disulfide. In addition, these studies confirmed that it is possible to distinguish the different x‐ray crystal structures from the solid‐state NMR experiment. Copyright © 1990 John Wiley & Sons, Ltd.