Solid-State NMR: Basic Principles and Practice

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· Momentum Press
Ebook
292
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About this ebook

The power of nuclear magnetic resonance, NMR, for characterizing molecules dissolved in solution is widely acknowledged. However, the application of NMR to the solid state is much less well appreciated. This book sets out the fundamental principles of solid-state NMR, explaining how NMR in solids differs from that in solution, and showing how the various interactions of NMR can be manipulated to yield high-resolution spectra and to give information on local structure and dynamics in solids.

Solid State NMR aims to take some of the mystique out of solid-state NMR by providing a comprehensible discussion of the methodology involved, including the basic concepts and practical guidance on the implementation of the experiments. A basic knowledge of solution-state NMR is assumed and is only briefly covered.

This book will be a valuable introduction and reference both for students and practicing scientists, as well as for non-experts interested in learning how NMR can be usefully applied to solid systems. Detailed mathematical treatments are delayed to a chapter at the mid-point of the text and can be skipped. Introductions to experiments and numerical simulations are provided to help link NMR results to experimental practice.

The different aspects of solid-state NMR, from basic pulse-and-acquire experiments to sophisticated techniques for the measurement of anisotropy information are presented, with examples chosen to illustrate the wide variety of applications of the technique, as well as its complementarity to other solid-state characterization techniques such as X-ray diffraction. Various aspects of NMR crystallography are covered as are topics of motion in solids.

The power of nuclear magnetic resonance, NMR, for characterizing molecules dissolved in solution is widely acknowledged. However, the application of NMR to the solid state is much less well appreciated. This book sets out the fundamental principles of solid-state NMR, explaining how NMR in solids...

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About the author

David C. Apperley studied chemistry at the University of East Anglia, Norwich, and gained a Ph.D. for research on dipolar coupling in solids from the Open University, Milton Keynes, in 1986. He further developed his interest in solid-state NMR while working as a senior experimental officer in the Durham Solid-State NMR Research Service, at first in the Industrial Research Laboratories and now in the Department of Chemistry, Durham University. For many years he has been the manager of the facility, which serves both industry and other universities (the latter operation funded by the Engineering and Physical Sciences Research Council). His role with the NMR Service is to provide access to, training in, and interpretation of results from solid-state NMR measurements for scientists in industry and in the UK universities. As well as providing support to organic, organometallic, inorganic, and physical chemists, he specializes in the experimental application of solid-state NMR techniques to characterization or problem solving in a wide range of solid (and sometimes not so solid) materials, including pharmaceuticals, catalysts, ceramics and glasses, polymers (synthetic and natural), soils (and related materials), and household products. He has coauthored 150 publications in the scientific literature.

Robin K. Harris is an emeritus professor at the University of Durham, UK, where he previously served as professor of chemistry, head of the Physical and Theoretical Chemistry section, and chairman of the Chemistry Department. He obtained his first degree from Cambridge University and undertook research in NMR there, supervised by Norman Sheppard, for his Ph.D. After 2 years as a postdoctoral fellow at the Mellon Institute, Pittsburgh, he joined the (then new) University of East Anglia (Norwich, UK) as a lecturer, winning promotion to a readership and then obtaining a personal chair. He moved to the University of Durham in 1984. His early research was on solution-state NMR, but, starting in 1976, he has carried out pioneering research in solid-state NMR, using cross-polarization and magic-angle spinning, for a wide variety of elements and in an extensive range of chemical systems, including organometallics, polymers, ceramics, and inorganics. In the last 20 years, much research has been directed toward problems involving pharmaceutical compounds and systems, especially relating to polymorphism and quantitative studies. Current interests center around the concept of “NMR crystallography” and include both sophisticated NMR experimental methods and computations of chemical shifts using crystallographic repetition. Professor Harris was awarded an Sc.D. degree by Cambridge University for his research in 1978. He is a Fellow of the Royal Society of Chemistry and has won its awards in Chemical Instrumentation (1985) and in Analytical Spectroscopy (1998). He was the director of the UK National Research Service in Solid-State NMR (1986–2004). He has been an author of over 500 research articles, mostly on NMR, and has acted as author or editor of several books on the subject. He is the senior editor-in-chief of the Encyclopedia of Magnetic Resonance.

Paul Hodgkinson studied chemistry at Queen’s College, Oxford, completing his PhD in 1995 on the sampling of NMR data. His interests in solid-state NMR developed during postdoctoral research at UC Berkeley (Royal Society/NATO fellowship with Professor Alex Pines) and at the Ecole Normale Supérieure de Lyon (Marie-Curie fellowship with Professor Lyndon Emsley). He was appointed to a research fellowship in the Chemistry Department, University of Durham, UK, in 1998 and is currently a reader in magnetic resonance at Durham, where he directs the Durham Solid-State NMR Research Service. His research combines interests in technique development and methodology in solid-state NMR as well as applications to chemical problems. His group develops NMR theory and numerical simulation software to explore the dynamics of large coupled spin systems and applies solid-state NMR in the area of structural chemistry, particularly of systems with mobility such as soft solids and solvates, and to pharmaceutical solids. A particular interest is in combining information from diffraction-based experiments, NMR and computation of NMR parameters (using DFT codes), and dynamics (molecular dynamics simulations). He has authored/coauthored over 60 research articles in the area of NMR.

David C. Apperley studied chemistry at the University of East Anglia, Norwich, and gained a Ph.D. for research on dipolar coupling in solids from the Open University, Milton Keynes, in 1986. He further developed his interest in solid-state NMR while working as a senior experimental officer in the...

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