Solid-State ⁷⁷Se NMR of Organoselenium Compounds through Cross Polarization Magic Angle Spinning (CPMAS) Method

Characterization of selenium states by ⁷⁷Se NMR is quite important to provide vital information for mechanism studies in organoselenium-catalyzed reactions. With the development of heterogeneous polymer-supported organoselenium catalysts, the solid state ⁷⁷Se NMR comes to the spotlight. It is necessary to figure out an advanced protocol that provides good quality spectra within limited time because solid state ⁷⁷Se NMR measurements are always time consuming due to the long relaxation time and the relatively low sensitivity. Studies on small molecules and several novel polymer-supported organoselenium materials in this article showed that cross polarization (CP) method with the assistance of magic angle spinning (MAS) was more efficient to get high quality spectra than the methods by using single pulse (SP) or high power ¹H decoupling (HPHD) combined with MAS. These results lead to a good understanding of the effect of the molecular structure, the heteronuclear coupling, the long-range ordering of the solid (crystal or amorphous), and the symmetry of ⁷⁷Se on quality of their spectra.