Download or read book Solid state NMR Techniques for Dipolar Coupling Measurements in Locally ordered Biological Solids written by Rebecca Ann Shapiro and published by . This book was released on 2011 with total page 48 pages. Available in PDF, EPUB and Kindle. Book excerpt: In the low-viscosity samples used in solution-state nuclear magnetic resonance (NMR) spectroscopy, molecular tumbling occurs on a much faster timescale than a single NMR experiment. As a result, anisotropic interactions between the nuclei average to zero and sharp, narrow, isotropic lineshapes are easily obtained. However, in systems with local order, rotational and translation mobility of molecules is signifcantly reduced. In this solid-state regime, anisotropic interactions are no longer motionally averaged, and three additional effects are observed to severely complicate NMR spectra: heteronuclear and homonuclear dipolar couplings, and chemical shift anisotropy (CSA). Magic-angle spinning (MAS) is a solid-state NMR (ssNMR) technique that makes it possible to mechanically average these anisotropic effects to zero and acquire sharp, isotropic peaks analogous to those found in solution. However, the presence of dipolar couplings and CSA allows additional structural information about biomolecules to be extracted; so there is demand for ssNMR techniques that take advantage of anisotropic interactions. Switched angle spinning (SAS) is one such method that can be used for structural studies of oriented biological samples. SAS combines the advantage of the magic angle spinning with the structural information provided by heteronuclear and homonuclear dipolar couplings and CSA by correlating isotropic chemical shifts in one dimension with anisotropic information in a second dimension. Presented herein is current work on two related research efforts: the development and characterization of a new biologically-relevant alignment medium with increased thermal stability ideal for recovery of additional structural constraints from dipolar couplings and CSA in membrane proteins and peptides, and simulation work laying the foundation for new SAS experiments optimized for structural studies of membrane proteins, peptides, and other biomolecules with local order induced by bicelles or other liquid-crystalline alignment media.
Download or read book Solid and Solution state NMR Techniques for the Investigation of Local Ordering in Membrane derived Solids Via Measurement of Scaled Dipolar Couplings written by Rebecca Shapiro Celik and published by . This book was released on 2013 with total page 139 pages. Available in PDF, EPUB and Kindle. Book excerpt: In the low-viscosity samples used in solution-state nuclear magnetic resonance (NMR) spectroscopy, molecular tumbling occurs on a much faster timescale than a single NMR experiment. As a result, anisotropic interactions between the nuclei average to zero; and sharp, narrow, isotropic lineshapes are easily obtained. However, in systems with local order, rotational and translation mobility of molecules is significantly reduced. In this solid-state regime, anisotropic interactions are no longer motionally averaged, and three additional effects are observed that can severely complicate NMR spectra: heteronuclear and homonuclear dipolar couplings, and chemical shift anisotropy (CSA). Magic-angle spinning (MAS) is a solid-state NMR (ssNMR) technique that makes it possible to mechanically average these anisotropic effects to zero and acquire sharp, isotropic peaks analogous to those found in solution. However, the presence of dipolar couplings and CSA allows additional structural information about biomolecules to be extracted; so there is demand for NMR techniques that take advantage of anisotropic interactions. Alignment media, such as bicelle mixtures, are used to introduce a controllable degree of anisotropy for the purpose of collecting scaled dipolar couplings in ssNMRand residual dipolar couplings (RDCs) in solution state, and their composition can be tailored to optimize the degree of order they impose and therefore the degree to which dipolar couplings and other anisotropic interactions are motionally averaged. Altering the composition of an alignment medium can also influence the temperature range over which an aligned phase exists, which is beneficial in dealing with temperature sensitive biomolecules. Switched-angle spinning (SAS) is another NMR method aimed at analyzing anisotropic interactions in the structural studies of oriented biological solids. SAS combines the advantages of the magic angle spinning with the structural information provided by heteronuclear and homonuclear dipolar couplings and CSA by correlating isotropic chemical shifts in one dimension with anisotropic information in a second dimension. Finally, symmetry-based pulse sequences introduce sophisticated spin-space selection rules into MAS experiments that allow for reintroduction of only specific NMR interactions while suppressing others. Presented herein is current work on three related research efforts: the development and characterization of a new biologically-relevant alignment medium with increased thermal stability ideal for recovery of additional structural constraints from dipolar couplings and CSA in membrane proteins and peptides; simulation work and preliminary experiments laying the foundation for new variable-angle spinning (VAS) and switched-angle spinning (SAS) experiments optimized for structural studies of membrane proteins, peptides, and other biomolecules with local order induced by bicelles or other liquid-crystalline alignment media; and an investigation of an unusual chlorosulfolipid membrane component via a proton-detected local field experiment that utilizes a symmetry-based pulse sequence to selectively recouple heteronuclear dipolar couplings and CSA while prohibiting evolution of J-coupling, chemical shift, and homonuclear dipolar couplings.
Download or read book Perspectives on Solid State NMR in Biology written by S.R. Kiihne and published by Springer Science & Business Media. This book was released on 2013-03-14 with total page 227 pages. Available in PDF, EPUB and Kindle. Book excerpt: Solid state NMR is rapidly emerging as a universally applicable method for the characterization of ordered structures that cannot be studied with solution methods or diffraction techniques. This proceedings -; from a recent international workshop - captures an image of the latest developments and future directions for solid state NMR in biological research, particularly on membrane proteins. Detailed information on how hormones or drugs bind to their membrane receptor targets is needed, e.g. for rational drug design. Higher fields are bringing clear improvements, and the power of solid state NMR techniques for studying amorphous and membrane associated peptides, proteins and complexes is shown by examples of applications at ultra-high fields. Progress in protein expression, experimental design and data analysis are also presented by leaders in these research areas.
Download or read book Modern Methods in Solid state NMR written by Paul Hodgkinson and published by Royal Society of Chemistry. This book was released on 2018-04-05 with total page 452 pages. Available in PDF, EPUB and Kindle. Book excerpt: 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.
Download or read book Solid State NMR IV Methods and Applications of Solid State NMR written by B. Blümich and published by Springer Science & Business Media. This book was released on 2012-12-06 with total page 210 pages. Available in PDF, EPUB and Kindle. Book excerpt: Solid-State NMR is a branch of Nuclear Magnetic Resonance which is presently experiencing a phase of strongly increasing popularity. The most striking evidence is the large number of contributions from Solid-State Resonance at NMR meetings, approaching that ofliquid state resonance. Important progress can be observed in the areas of methodological developments and applications to organic and inorganic matter. One volume devoted to more or less one of each of these areas has been published in the preceding three issues. This volume can be considered an addendum to this series. Selected methods and applications of Solid-State NMR are featured in three chapters. The first one treats the recoupling of dipolar interactions in solids, which are averaged by fast sample rotation. Following an introduction to effective Hamiltonians and Floquet theory, different types of experiment such as rotary resonance, dipolar chemical shift correlation spectroscopy, rotational resonance and multipulse recoupling are treated in the powerful Floquet formalism. In the second chapter, the different approaches to line narrowing of quadrupolar nuclei are reviewed in a. consistent formulation of double resonance (DaR) and dynamic angle spinning (DAS). Practical aspects of probe design are considered as well as advanced 2D experiments, sensitivity enhancement techniques, and spinning sideband manipulations. The use of such techniques dramatically increases the number of nuclei which can be probed in high resolution NMR spectroscopy. The final chapter describes new experimental approaches and results of structural studies of noncrystalline solids.
Download or read book Solid State NMR Studies of Biopolymers written by Anne E. McDermott and published by John Wiley & Sons. This book was released on 2012-12-19 with total page 596 pages. Available in PDF, EPUB and Kindle. Book excerpt: The content of this volume has been added to eMagRes (formerly Encyclopedia of Magnetic Resonance) - the ultimate online resource for NMR and MRI. The field of solid state NMR of biological samples [ssNMR] has blossomed in the past 5-10 years, and a cohesive overview of the technology is needed for new practitioners in industry and academia. This title provides an overview of Solid State NMR methods for studying structure dynamics and ligand-binding in biopolymers, and offers an overview of RF pulse sequences for various applications, including not only a systematic catalog but also a discussion of theoretical tools for analysis of pulse sequences. Practical examples of biochemical applications are included, along with a detailed discussion of the many aspects of sample preparation and handling that make spectroscopy on solid proteins successful. About EMR Handbooks / eMagRes Handbooks The Encyclopedia of Magnetic Resonance (up to 2012) and eMagRes (from 2013 onward) publish a wide range of online articles on all aspects of magnetic resonance in physics, chemistry, biology and medicine. The existence of this large number of articles, written by experts in various fields, is enabling the publication of a series of EMR Handbooks / eMagRes Handbooks on specific areas of NMR and MRI. The chapters of each of these handbooks will comprise a carefully chosen selection of articles from eMagRes. In consultation with the eMagRes Editorial Board, the EMR Handbooks / eMagRes Handbooks are coherently planned in advance by specially-selected Editors, and new articles are written (together with updates of some already existing articles) to give appropriate complete coverage. The handbooks are intended to be of value and interest to research students, postdoctoral fellows and other researchers learning about the scientific area in question and undertaking relevant experiments, whether in academia or industry. Have the content of this Handbook and the complete content of eMagRes at your fingertips! Visit: www.wileyonlinelibrary.com/ref/eMagRes View other eMagRes publications here
Download or read book Current Developments in Solid State NMR Spectroscopy written by Norbert Müller and published by Springer Science & Business Media. This book was released on 2003-01-31 with total page 154 pages. Available in PDF, EPUB and Kindle. Book excerpt: 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.
Download or read book Separated Local Field NMR Spectroscopy In Partially Ordered Systems New Methodologies And Applications written by and published by . This book was released on 2004 with total page pages. Available in PDF, EPUB and Kindle. Book excerpt: Dipolar couplings are one of the major source of structural information. Due to their dependence on the distance between the nuclei and the angle of orientation of the dipolar vector with respect to the magnetic field, they provide significant insight into the geometry and topology of molecules. As the dipolar interactions are in general present in the solid phase of the compounds, solid state NMR experiments have gained significant popularity and is widely used. Separated Local Field NMR spectroscopy based on cross-polarization technique has been used to measure the heteronuclear dipolar couplings in solid state. However, the technique undergoes many experimental challenges and requires further development. This thesis is concerned mainly with the development of techniques to measure the dipolar couplings accurately in oriented molecules. In this regard, a method for fast data acquisition is also proposed. The first chapter briefly introduces the basics of NMR spectroscopy, methodologies applied for obtaining a high resolution NMR spectrum in the solid state. An introduction to liquid crystals is presented and the nature of NMR interaction in the liquid crystalline phases is described. In chapter-2, a new pulse scheme has been proposed that includes the X-nucleus polarization in the SLF experiments and is shown to provide better sensitivity and resolution. A quantitative analysis with simulation and experimental results are also presented. In chapter-3, the performance of various homonuclear decoupling pulse schemes incorporated into SLF experiments tested on oriented systems are compared. The proposed pulse schemes are shown to provide high resolution spectrum with accurate dipolar coupling measurement for natural abundant samples and for uniformly labeled compounds as well. Theoretical description with simulation and experimental results shown here are found to provide optimum results under several technical complications seen with respect to the conventional met.
Download or read book Nmr Spectroscopy of Biological Solids written by A. Ramamoorthy and published by CRC Press. This book was released on 2019-08-30 with total page 368 pages. Available in PDF, EPUB and Kindle. Book excerpt: Over the past decade, a myriad of techniques have shown that solid-state nuclear magnetic resonance (NMR) can be used in a broad spectrum of applications with exceptionally impressive results. Solid-state NMR results can yield high-resolution details on the structure and function of many important biological solids, including viruses, fibril-forming molecules, and molecules embedded in the cell membrane. Filling a void in the current literature, NMR Spectroscopy of Biological Solids examines all the recent developments, implementation, and interpretation of solid-state NMR experiments and the advantages of applying them to biological systems. The book emphasizes how these techniques can be used to realize the structure of non-crystalline systems of any size. It explains how these isotropic and anisotropic couplings interactions are used to determine atomic-level structures of biological molecules in a non-soluble state and extrapolate the three-dimensional structure of membrane proteins using magic-angle spinning (MAS). The book also focuses on the use of multidimensional solid-state NMR methods in the study of aligned systems to provide basic information about the mechanisms of action of a variety of biologically active molecules. Addressing principles, methods, and applications, this book provides a critical selection of solid-state NMR methods for solving a wide range of practical problems that arise in both academic and industrial research of biomolecules in the solid state. NMR Spectroscopy of Biological Solids is a forward-thinking resource for students and researchers in analytical chemistry, bioengineering, material sciences, and structural genomics.
Download or read book Solid State NMR Spectroscopy written by Melinda J. Duer and published by John Wiley & Sons. This book was released on 2008-04-15 with total page 592 pages. Available in PDF, EPUB and Kindle. Book excerpt: This book is for those familiar with solution-state NMR who are encountering solid-state NMR for the first time. It presents the current understanding and applications of solid-state NMR with a rigorous but readable approach, making it easy for someone who merely wishes to gain an overall impression of the subject without details. This dual requirement is met through careful construction of the material within each chapter. The book is divided into two parts: "Fundamentals" and "Further Applications." The section on Fundamentals contains relatively long chapters that deal with the basic theory and practice of solid-state NMR. The essential differences and extra scope of solid-state NMR over solution-state is dealt with in an introductory chapter. The basic techniques that all chapters rely on are collected into a second chapter to avoid unnecessary repetition later. Remaining chapters in the "Fundamentals" part deal with the major areas of solid-state NMR which all solid-state NMR spectroscopists should know about. Each begins with an overview of the topic that puts the chapter in context. The basic principles upon which the techniques in the chapter rely are explained in a separate section. Each of these chapters exemplifies the principles and techniques with the applications most commonly found in current practice. The "Further Applications" section contains a series of shorter chapters which describe the NMR techniques used in other, more specific areas. The basic principles upon which these techniques rely will be expounded only if not already in the Fundamentals part.
Download or read book Transient Techniques in NMR of Solids written by Bernard C. Gerstein and published by . This book was released on 1985 with total page 320 pages. Available in PDF, EPUB and Kindle. Book excerpt: This volume is an ideal starting point for the graduate student seeking a basic introduction to the theory and uses of solid-state nuclear magnetic resonance (NMR) spectroscopy. Accessible to students with only a survey-level physics background, the material assumes little prior knowledge of the basic theory of electromagnetism. All the major areas are covered, including an introduction to concepts of time-dependent quantum mechanics as they apply to NMR spectroscopy of the solid state. Each chapter includes problems designed to enhance the reader's understanding of the material. Instructive and practical, this volume provides the basic knowledge needed to access the general literature and the more advanced monographs on this subject. In addition to assisting entrance into the field, Transient Techniques in NMR of Solids will be a useful guide for professionals already working in related areas of chemistry. FROM THE PREFACE: Nuclear magnetic resonance (NMR) is truly a remarkable phenomenon. Remarkable can imply different things to different people. From the point of view of a physicist, spin dynamics is an elegant example of the use of time-dependent quantum mechanics, and NMR absorption of energy is a prototype for spectroscopic transitions. From the point of view of the practicing chemist and materials scientist, NMR spectroscopy is an invaluable tool for the identification of chemical species and structures. Had NMR spectroscopic techniques commercially available in the early 1960s been the only result of investigations of this phenomenon, it would have had a major impact on the course of chemical analysis. The study of liquids and solutions for chemical shifts and couplings of protons had produced a rapid means of identifying chemical species nondestructively. The study of dynamical properties also could be addressed by study of temperature dependence of the spectra or of the saturation of the resonance by high-power irradiation. Even at that time, however, studies of the spin dynamics had already begun to indicate that there were many interesting facets of the NMR phenomenon left to exploit. For example, the Fourier-transform relationship of the free-induction decay and the absorption spectrum had been shown and the basis of the cross-polarization experiment was being investigated. A number of chemists had begun to study the spin*b1lattice relaxation times of species by pulse NMR techniques by utilizing methods that were not familiar at that time to the typical chemist but that are now commonly employed in NMR analysis. The principal characteristic of the NMR technique that makes it so useful for chemical analysis of liquids and solutions is the high resolution that allows one to observe very small interactions such as the chemical shift and the spin*b1spin coupling. These weak interactions are quite sensitive to the local environment of the spin and therefore may be used as a diagnostic for the environment. The connectivity of chemical structure is often mimicked closely in the NMR connectivity of the spectrum, and quantitative informaton is relatively easy to obtain. Nuclear magnetic resonance spectra of solids exhibit such resolution only in special cases. The primary (although not the exclusive) reason for the lack of resolution in the spectrum of a typical solid is the presence of the dipole*b1dipole interaction, which dominates the NMR spectroscopy of solids that have been of interest to chemists. One solution (no pun intended) to the problem of obtaining chemical-shift information about such solids is to dissolve them and to study them in solution. However, if the solid is insoluble or otherwise intractable or if the analysis involves questions about the properties of the substance in the solid state, then there arises a need for techniques to study the weaker interactions in the presence of the dipole*b1dipole interaction or other overwhelming interactions. This volume describes the means dev
Download or read book Solid State NMR written by Jerry C. C. Chan and published by Springer Science & Business Media. This book was released on 2011-10-26 with total page 328 pages. Available in PDF, EPUB and Kindle. Book excerpt: Dipolar Recoupling, by Niels Chr. Nielsen, Lasse A. Strassø and Anders B. Nielsen.- Solid-State NMR Techniques for the Structural Determination of Amyloid Fibrils, by Jerry C. C. Chan.- Solid-State 19F-NMR of Peptides in Native Membranes, by Katja Koch, Sergii Afonin, Marco Ieronimo, Marina Berditsch and Anne S. Ulrich.- Probing Quadrupolar Nuclei by Solid-State NMR Spectroscopy: Recent Advances, by Christian Fernandez and Marek Pruski.- Solid State NMR of Porous Materials Zeolites and Related Materials, by Hubert Koller and Mark Weiß.- Solid-State NMR of Inorganic Semiconductors, by James P. Yesinowski.-
Download or read book Solid State NMR of Polymers written by T. Asakura and published by Elsevier. This book was released on 1998-08-03 with total page 1017 pages. Available in PDF, EPUB and Kindle. Book excerpt: In polymer science and technology, the advanced development of various new polymer materials with excellent properties and functions is desirable. For this purpose it is necesary to determine the exact relationship between physical properties and molecular structure-dynamics with powerful techniques. One such technique is solid state NMR. Recently, high resolution NMR studies of solids have been realized by using advanced pulse and mechanical techniques, which has resulted in a variety of structural and dynamical information on polymer systems. Solid state NMR has provided characteristic information which cannot be obtained by other spectroscopic methods.This book is divided into two parts. The first part covers the principles of NMR, important NMR parameters such as chemical shifts, relaxation times, dipolar interactions, quadrupolar interactions, pulse techniques and new NMR methods. In the second part, applications of NMR to a variety of polymer systems in the solid state are described.Features of this book:• Contains an up-to-date and comprehensive account of solid state NMR of polymers by leading researchers in the field• Provides a compilation of solid state NMR of polymers, which makes it an ideal reference book for both NMR researchers and general polymer scientists.This book will be of interest to the NMR community, and will be invaluable for both the beginner and the expert.
Download or read book New Techniques in Solid State NMR written by Jacek Klinowski and published by Springer Science & Business Media. This book was released on 2004-12-10 with total page 372 pages. Available in PDF, EPUB and Kindle. Book excerpt: With contributions by numerous experts
Download or read book Solid State NMR in Materials Science written by Vladimir I. Bakhmutov and published by CRC Press. This book was released on 2016-04-19 with total page 277 pages. Available in PDF, EPUB and Kindle. Book excerpt: Solid-state NMR is a powerful physical method widely applied in modern fundamental and applied science, medicine, and industry. Its role is particularly valuable in materials chemistry due to the capability of solid-state NMR to rapidly solve tasks connected with structural descriptions of complex systems on macro and/or molecular levels, and the i
Download or read book Solid State NMR III Organic Matter written by Bernhard Blümich and published by Springer. This book was released on 1994-11-04 with total page 232 pages. Available in PDF, EPUB and Kindle. Book excerpt: Solid-State NMR is a branch of Nuclear Magnetic Resonance which is presently experiencing a phase of strongly increasing popularity. The most striking evidence is the large number of contributions from Solid-State Resonance atNMR meetings, approaching that ofliquid state resonance. Important progress can be observed in three areas: Methodological developments, applications to inorganic matter, and applications to organic matter. These developments are intented to be captured in three volumes in this series, each of them being devoted to more or less one of these areas. The present volume on Solid-State NMR III is devoted mainly to organic matter. The recent developments of deuteron NMR and their applications are reviewed in the first chapter. Crosspolarization, MAS, and dynamic angle spinning are being explored for enhancement of information and sensitivity. In addition to the analysis of classical relaxation times and modern 2D spectra, detailed dynamic information becomes accessible from investigations of the relaxation time anisotropies. The second chapter examines cross-polarization in static and rotating solids under conditions of spin diffusion and thermal motion. The underlying dipole-dipole interaction is further exploited by the techniques described in the third chapter for studies of polymer-polymer miscibility. Short range techniques are discriminated from long-range techniques based on spin diffusion. The use ofthese techniques is illustrated by a case study ofPMMAJPVF blends. The last chapter addresses novel z methods and applications of two-dimensional exchange NMR for investigations of relative molecular orientations, polymer morphology, molecular dynamics, and macroscopic molecular order.
Download or read book Solid State NMR Methods and applications of solid state NMR written by Bernhard Blümich and published by Springer. This book was released on 1994 with total page 224 pages. Available in PDF, EPUB and Kindle. Book excerpt:
