Structure and dynamics of bis(organothiophosphoryl) disulfides in the solid state. X-Ray diffraction and cross-polarization magic angle spinning nuclear magnetic resonance studies

摘要: The structure and dynamics of selected bis(organothiophosphoryl) disulfides have been studied by single-crystal X-ray diffraction high-resolution solid-state NMR spectroscopy. crystal molecular structures bis[tert-butyl(phenyl)thiophosphoryl] disulfide 1, bis-(diphenoxythiophosphoryl) 2 bis[tert-butyl(methoxy)thiophosphoryl] 3 were determined, giving space groups C2/c, P212121 P for 3, respectively. Both phosphorus centres the 1 same absolute configuration, as those although their environments significantly different. It has unambiguously proved that S–S bond length varies a function PSSP torsional angle. Moreover influence S–S–PS conformation on P–S is discussed. Carbon-13 dipolar-dephasing experiments, using powdered samples, indicated both tert-butyl methoxy attached to atom in fast regime exchange.