NMR crystallography: structure and properties of materials from solid-state nuclear magnetic resonance observables.

David L Bryce

doi:10.1107/s2052252517006042

Abstract

This topical review provides a brief overview of recent developments in NMR crystallography and related NMR approaches to studying the properties of molecular and ionic solids. Areas of complementarity with diffraction-based methods are underscored. These include the study of disordered systems, of dynamic systems, and other selected examples where NMR can provide unique insights. Highlights from the literature as well as recent work from my own group are discussed.

Highlights

From the early days of nuclear magnetic resonance (NMR), experiments on crystalline samples have provided structural and crystallographic information (Pake, 1948; Harris et al, 2009)
In this topical review article, I will provide a short survey of selected recent work in the field of NMR crystallography, a topic on which the IUCr established a Commission in 2014 (Report of the Executive Committee for 2014, 2016), as well as a broader look at various applications of NMR methods to studying the structure and properties of various solids
In the final category of NMR crystallographic approaches, NMR data may be used to select or cross-validate certain structures produced via other methods

Summary

Introduction

From the early days of nuclear magnetic resonance (NMR), experiments on crystalline samples have provided structural and crystallographic information (Pake, 1948; Harris et al, 2009). The information available in a particular case will depend on the nature of the sample, and may range from an internuclear distance to a complete structural model of a complex system such as a protein In this topical review article, I will provide a short survey of selected recent work in the field of NMR crystallography, a topic on which the IUCr established a Commission in 2014 (Report of the Executive Committee for 2014, 2016), as well as a broader look at various applications of NMR methods to studying the structure and properties of various solids. In the final category of NMR crystallographic approaches, NMR data (e.g. chemical shifts) may be used to select or cross-validate certain structures produced via other methods These other methods may include diffraction refinements and/or advanced computational methods such as crystal structure prediction (CSP) algorithms. Some of the examples from my laboratory which will be described include (i) a multinuclear magnetic resonance structure refinement protocol based on experimental and computed electric field gradient (EFG) tensors, (ii) insights into noncovalent interactions, such as halogen bonds, via combined X-ray and NMR studies, and (iii) novel insights into crystallographic symmetry, as well as molecular dynamics, via two-dimensional J-resolved NMR experiments

Solid-state NMR basics

Applications and examples

Findings

Concluding remarks