Solid-state nuclear magnetic resonance (SSNMR) is a powerful tool for the study of chemical structure and dynamics. The interactions that manifest in NMR spectra are anisotropic (id est, orientation dependent) in origin, often resulting in inhomogeneous broadening that can yield spectra exceeding circa 250 kHz in breadth; such spectra are often referred to as ultra-wideline (UW) NMR spectra. In many cases, UWNMR spectra cannot be acquired using conventional methods and rectangular radiofrequency (RF) pulses - rather, specialized pulses and techniques must be implemented. Furthermore, the large suite of high-resolution methods based on magic-angle spinning (MAS) are generally unsuitable for the acquisition of UWNMR spectra. Frequency-swept (FS) pulses are amplitude- and phase-modulated pulses that can irradiate NMR frequencies over large bandwidths. One of these is the wideband uniform-rate smooth-truncation (WURST) pulse, which features a linear effective frequency sweep. WURST pulses are used in the WURST-Carr-Purcell/Meiboom-Gill (WURST-CPMG) and broadband adiabatic inversion-cross polarization (BRAIN-CP) pulse sequences, which have been shown to be effective for the acquisition of UWNMR spectra of stationary (static) samples. These sequences have limitations, and to date, their capabilities have not been fully explored, nor have they been described from a theoretical point of view in a comprehensive manner.Signal processing is an integral component of pulsed-Fourier transform NMR spectroscopy, and comprises many protocols for enhancing spectral sensitivity and resolution. There has been much interest in advanced spectral processing methods such as alternate basis transformations (id est, besides Fourier encoding), statistical analyses (e.g., singular value decomposition, SVD, and principal component analysis, PCA), numerical regression (e.g., non-negative least squares), and the use of deep learning and neural networks. Such methodologies are now routinely implemented in imaging and multidimensional solution NMR, but are seldom explored in SSNMR. This thesis describes the development of new methods for the acquisition and advanced processing of conventional, wideline, and UW SSNMR spectra, including: (i) the design of new pulses and pulse sequences with optimal control theory (OCT); (ii) the modification of existing pulse sequences for UWNMR under MAS conditions; (iii) achieving signal enhancements with CPMG pulse sequences via the suppression of weak homonuclear dipolar coupling interactions under static and MAS conditions; (iv) the application of the BRAIN-CP pulse sequence to integer-spin nuclei, along with a thorough theoretical treatment; (v) rapid and robust measurements of longitudinal relaxation time constants (T1) and T1 anisotropies from UWNMR spectra under static conditions; (vi) the development and application of advanced processing methods for resolving UWNMR relaxation data with inverse Laplace transforms; and (vii) the development of a Python library for denoising 1D and 2D NMR spectra with SVD, PCA, and wavelet transforms. It is hoped that these methods will open up the Periodic Table of elements to increasingly routine exploration by SSNMR spectroscopy, aiding researchers in chemistry, biochemistry, materials science, and physics with advanced molecular-level characterization of their materials.

Solid-state NMR covers an enormous range of material types and experimental techniques. Although the basic instrumentation and techniques of solids NMR are readily accessible, there can be significant barriers, even for existing experts, to exploring the bewildering array of more sophisticated techniques. In this unique volume, a range of experts in different areas of modern solid-state NMR explain about their area of expertise, emphasising the “practical aspects” of implementing different techniques, and illustrating what questions can and cannot be addressed. Later chapters address complex materials, showing how different NMR techniques discussed in earlier chapters can be brought together to characterise important materials types. The volume as a whole focusses on topics relevant to the developing field of “NMR crystallography” – the use of solids NMR as a complement to diffraction crystallography. This book is an ideal complement to existing introductory texts and reviews on solid-state NMR. New researchers wanting to understand new areas of solid-state NMR will find each chapter to be the equivalent to spending time in the laboratory of an internationally leading expert, learning the hints and tips that make the difference between knowing about a technique and being ready to put it into action. With no equivalent on the market, it will be of interest to every solid-state NMR researcher (academic and postgraduate) working in the chemical sciences.

Solid State NMR A thorough and comprehensive textbook covering the theoretical background, experimental approaches, and major applications of solid-state NMR spectroscopy Nuclear Magnetic Resonance (NMR) spectroscopy is a powerful non-destructive technique capable of providing information about the molecular structure and dynamics of molecules. Alongside solution-state NMR, a well-established technique to study chemical structures and investigate physico-chemical properties of molecules in solutions, solid-state NMR (SSNMR) offers many exciting possibilities for the analysis of solid and soft materials across scientific fields. SSNMR shows unique capabilities for a detailed investigation of structural and dynamic properties of materials over wide space and time ranges. For this reason, and thanks to significant advances in the past several years, the application of SSNMR to materials is rapidly increasing in disciplines such as chemistry, physics, and materials and life sciences. Solid State NMR: Principles, Methods, and Applications offers a systematic introduction to the theory, methodological concepts, and major experimental methods of SSMR spectroscopy. Exploring the unique potential of SSNMR for the structural and dynamic characterization of soft and either amorphous or crystalline solid materials, this comprehensive textbook provides foundational knowledge and recent developments of SSNMR, covering physical and theoretical background, experimental methods, and applications to pharmaceuticals, polymers, inorganic and hybrid materials, liquid crystals, and model membranes. Written by two expert authors to ensure a clear and consistent presentation of the subject, this textbook: Includes a brief introduction to the historical aspects and broad theoretical background of solid-state NMR spectroscopy Provides helpful illustrations to explain the various SSNMR concepts and methods Features accessible descriptive text with self-consistent use of quantum mechanics Covers the experimental aspects of SSNMR spectroscopy and in particular a description of many useful pulse sequences Contains references to relevant literature Solid State NMR: Principles, Methods, and Applications is the ideal textbook for university courses on SSNMR, advanced spectroscopies, and a valuable single-volume reference for spectroscopists, chemists, and researchers in the field of materials.

This book presents some of the latest developments in solid state NMR with potential applications in both materials and biological science. The main emphasis is on a strong link between theory and experiment via numerical simulation of NMR spectra which play a pivotal role in the design and development of pulse schemes in solid state NMR. The papers focus on non-biological topics of solid state NMR spectroscopy making the book useful for scientists and advanced students in chemistry, physics, and materials science striving for deeper understanding of this topic and its application potential. Three invited reviews focus on developments in solid state NMR of quadrupolar nuclei, which are of high interest in areas like materials science and heterogeneous catalysis.

With contributions by numerous experts