Quantitative structure parameters from the NMR spectroscopy of quadrupolar nuclei

Abstract

AbstractNuclear magnetic resonance (NMR) spectroscopy is one of the most important characterization tools in chemistry, however, 3/4 of the NMR active nuclei are underutilized due to their quadrupolar nature. This short review centers on the development of methods that use solid-state NMR of quadrupolar nuclei for obtaining quantitative structural information. Namely, techniques using dipolar recoupling as well as the resolution afforded by double-rotation are presented for the measurement of spin–spin coupling between quadrupoles, enabling the measurement of internuclear distances and connectivities. Two-dimensional J-resolved-type experiments are then presented for the measurement of dipolar and J coupling, between spin-1/2 and quadrupolar nuclei as well as in pairs of quadrupolar nuclei. Select examples utilizing these techniques for the extraction of structural information are given. Techniques are then described that enable the fine refinement of crystalline structures using solely the electric field gradient tensor, measured using NMR, as a constraint. These approaches enable the solution of crystal structures, from polycrystalline compounds, that are of comparable quality to those solved using single-crystal diffraction.