PHOSPHORUS CHEMICAL-SHIFT TENSORS IN DITHIADIPHOSPHETANE DISULFIDES DETERMINED BY SOLID-STATE P-31 NUCLEAR-MAGNETIC-RESONANCE

The phosphorus chemical shift tensors of two dithiadiphosphetane disul fides, phenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (1) and ylth io)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (2), have been characte rized by solid-state P-31 nuclear magnetic resonance (NMR) measurement s. The weak homonuclear dipolar interaction between the two P-31 nucle i in each of these compounds has a significant influence on the P-31 N MR line shapes of static powder samples. From the weak dipolar splitti ngs it is possible to deduce the orientation of the phosphorus chemica l shift tenser. In both compounds, the intermediate components of the phosphorus chemical shift tensors, delta(22), were found to be perpend icular to the plane defined by the two phosphorus atoms and the two te rminal sulphur atoms in the molecule, S=P ... P=S. The smallest shift components, delta(33), were found to deviate approximately 14 degrees from the P=S bond direction.