Download or read book The Development of Proton Detection Based Paramagnetic Solid state NMR Methods as a General Structural Biology Tool written by Justin K. Thomas and published by . This book was released on 2022 with total page 0 pages. Available in PDF, EPUB and Kindle. Book excerpt: Determination of high-resolution three-dimensional structures of biological macromolecules is essential to studying their physiological functions. In recent years direct proton detection based magic angle spinning solid-state NMR has emerged as a widely applicable atomic-resolution structural tool that permits structure and dynamics studies of biological systems that are challenging for the usual structural techniques such as cryo-electron microscopy, X-ray crystallography, and solution-state NMR. In spite of remarkable recent progress in the accurate structural elucidation of biosystems, the widespread application of solid-state NMR for structural studies of large biosystems is hampered due to the dearth of unambiguous long-distance structural restraints. The conventional solid-state NMR approaches rely on upon through space 13C-13C and 13C-15N magnetic dipole-dipole coupling measurement to obtain structural restraints, which become vanishingly small for distances in the 5-6 Å regime and beyond. The paucity of long-range restraints from traditional through space dipolar coupling measurement-based approaches can be circumvented by site-specific incorporation of paramagnetic center to modified locations of a natively diamagnetic protein using a covalently bound paramagnetic tag. The introduction paramagnetic center in the diamagnetic system leads to the generation of large electron-nuclear hyperfine coupling interactions – which manifest themselves in NMR spectra as pseudocontact shifts (PCSs) and paramagnetic relaxation enhancement (PREs). The measurement of the magnitude of the electron-nuclear interactions can be used to obtain long-distance structural restraints for high-resolution structure calculation. In the solution state, PCSs and PREs measurements have been extensively utilized as long-range structural restraints for the analysis of the structure and interactions of biological macromolecules. However, the widespread applications of PCSs and PREs in solid-state NMR for structural studies have been limited because of the unavailability of compact non-native tags that can rigidly incorporate a paramagnetic metal center into protein in a residue-specific manner. In this thesis, we combined paramagnetic solid-state NMR approaches and proton detection-based solid-state NMR experiments to develop new solid-state NMR methodologies for the structural investigation of biomacromolecules. In chapter 1, we describe basic theoretical concepts of solid-state NMR, paramagnetic solid-state NMR, and direct proton detection-based pulse schemes. In chapter 2, we discuss the Pseudocontact shifts (PCSs) measurements in a natively diamagnetic protein using proton-detected solid-state NMR spectroscopy facilitated by Co2+ binding tag. The compact and rigid tag restricted the mobility of the metal in the solid phase by two-point attachment. In chapter 3, we describe a new method developed for measuring PREs restraints from aliphatic side-chain regions of the natively diamagnetic protein. We utilized new developed metal binding tag and reduced adjoining protonation (RAP) isotopic labeling strategy to site-specific measure side-chain PREs. In chapter 4, we applied direct proton detection-based sequential assignment experiments and radiofrequency driven dipolar recoupling (RFDR) schemes for structural investigation of Gerstmann-Straüssler-Scheinker (GSS) disease-associated Y145Stop human prion protein amyloids.
Download or read book Development of Solid state NMR Methodologies for Protein Structure Determination Based on Paramagnetic Tagging written by Dwaipayan Mukhopadhyay and published by . This book was released on 2018 with total page pages. Available in PDF, EPUB and Kindle. Book excerpt: In recent years solid-state NMR has emerged as a valuable tool for elucidating structure and dynamics of large biomolecular systems, especially suited for application in systems ranging from amyloid fibrils, membrane proteins to large protein ligand complexes inaccessible by more traditional structure determination techniques e.g. X-ray crystallography and solution-state NMR. Essential in determination of a biomolecular structure is the acquisition of numerous high quality interatomic distance restraints. However, conventional dipolar coupling based methods lead to significant challenges for accurate determination of critical long range distances. An alternative method to overcome this limitation is the incorporation of paramagnetic centers in proteins and utilization of the very large electron-nucleus couplings. In this dissertation, we combine state of the art proton-detection techniques with development of novel rigid transition metal binding tags, to improve the quality of long range distance restraints generated by measurement of site-specific paramagnetic relaxation enhancements in solid-state NMR.
Download or read book Paramagnetism in Experimental Biomolecular NMR written by Enrico Ravera and published by Royal Society of Chemistry. This book was released on 2018-08-06 with total page 340 pages. Available in PDF, EPUB and Kindle. Book excerpt: Paramagnetic NMR is a growing technique that represents an increasingly important tool for the investigation of biomolecules. This book presents an update and overview of the paramagnetic NMR phenomena and effects as well as guidelines for practical implementation of state-of-the-art experiments. All experiments are supported by a solid theoretical foundation. Areas mentioned are the development of solid state NMR, the use of paramagnetic tags providing information on the structure and mobility of the investigated systems, and dynamic nuclear polarization to increase sensitivity. Compiled by experts in the field, this book has international appeal for researchers as well as students interested in magnetic resonance and structural biology who require experimental support and accessible information.
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 2001-07-31 with total page 256 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 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 Solid State NMR Spectroscopy for Biopolymers written by Hazime Saitô and published by Springer Science & Business Media. This book was released on 2006-08-05 with total page 455 pages. Available in PDF, EPUB and Kindle. Book excerpt: ‘‘Biopolymers’’ are polymeric materials of biological origin, including globular, membrane, and fibrous proteins, polypeptides, nucleic acids, po- saccharides, lipids, etc. and their assembly, although preference to respe- ive subjects may be different among readers who are more interested in their biological significance or industrial and/or medical applications. Nevert- less, characterizing or revealing their secondary structure and dynamics may be an equally very important and useful issue for both kinds of readers. Special interest in revealing the 3D structure of globular proteins, nucleic acids, and peptides was aroused in relation to the currently active Structural Biology. X-ray crystallography and multidimensional solution NMR sp- troscopy have proved to be the standard and indispensable means for this purpose. There remain, however, several limitations to this end, if one intends to expand its scope further. This is because these approaches are not always straightforward to characterize fibrous or membrane proteins owing to extreme difficulty in crystallization in the former, and insufficient spectral resolution due to sparing solubility or increased effective molecular mass in the presence of surrounding lipid bilayers in the latter.
Download or read book High resolution Solid state NMR of Paramagnetic Molecules written by Gwendal Kervern and published by . This book was released on 2008 with total page 155 pages. Available in PDF, EPUB and Kindle. Book excerpt: This thesis is about high-resolution solid-state NMR of paramagnetic molecules. It exposes new methods to obtain high-resolution NMR spectra of paramagnetic solids. These methods gave us access to the structural information born by the electronic paramagnetism. In the first part, we propose new tools to overcome the difficulties associated with NMR of paramagnetic solids . These methods include proton to carbon magnetization transfer via dipolar recoupling, the use of adiabatic pulses with paramagnetic solids rotating at high MAS speeds, the development of a theory for a better understanding of the physics of such pulses. The second part exposes the interpretation of the high quality spectra obtained throught those methods. We characterized the electronic structure of high-spin iron (II) catalyst, we tackled the absence of the so-called "Curie relaxation" mechanism in the solid-state an we developed a new tool for crystallography thanks to proton NMR of paramagnetic powedrs.
Download or read book Biological NMR Spectroscopy written by John L. Markley and published by Oxford University Press. This book was released on 1997-01-30 with total page 375 pages. Available in PDF, EPUB and Kindle. Book excerpt: This book presents a critical assessment of progress on the use of nuclear magnetic resonance spectroscopy to determine the structure of proteins, including brief reviews of the history of the field along with coverage of current clinical and in vivo applications. The book, in honor of Oleg Jardetsky, one of the pioneers of the field, is edited by two of the most highly respected investigators using NMR, and features contributions by most of the leading workers in the field. It will be valued as a landmark publication that presents the state-of-the-art perspectives regarding one of today's most important technologies.
Download or read book Development and Application of New NMR Methods for Paramagnetic Inorganic Materials written by Kevin Sanders and published by . This book was released on 2018 with total page 0 pages. Available in PDF, EPUB and Kindle. Book excerpt: A precise understanding of the coordination geometry and electronic structure around metal cen- ters in catalysts and battery materials is crucial in order to control these complex systems, modify their behavior, and allow rational design of improved sites. However, such systems are not al- ways amenable for diffraction-based structural determination, and even if they are, obtaining atom-specific electronic structure can only be inferred indirectly from the atomic coordinates. As such, a direct probe of the electronic structure is highly desired. The aim of the present thesis is the investigation of structural and electronic properties of metal sites in catalysts and battery materials by magic-angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. MAS NMR is a powerful technique for the investigation of local effects in solid materials, and offers a direct probe of highly resolved electronic structures in paramagnetic solids. However, it suffers from limited sensitivity and resolution for nuclei lying close to a paramagnetic center in general. We address these limitations by first tackling some of the bottlenecks in the acquisition and interpretation of MAS NMR by developing and applying new methodologies to paramagnetic solids using ultra-fast (60-111) kHz MAS rates. A "toolkit" of suitably designed pulse sequences is assembled for broadband detection and interpretation of paramagnetic shifts in crystalline and non-crystalline solids. The potential of this methodology is explored for the elucidation of local geometry and electronic structure around paramagnetic metal sites in homogeneous and heterogeneous catalysts, and a set of mixed-phase Li-ion battery cathode materials. We anticipate that the approaches described herein form an essential tool to elucidate many outstanding questions about the structure and function of metal sites in modern chemistry.
Download or read book NMR of Proteins and Small Biomolecules written by Guang Zhu and published by Springer Science & Business Media. This book was released on 2012-03-28 with total page 255 pages. Available in PDF, EPUB and Kindle. Book excerpt: Application of NMR and Molecular Docking in Structure-Based Drug Discovery, by Jaime L. Stark and Robert Powers NMR as a Unique Tool in Assessment and Complex Determination of Weak Protein-Protein Interactions, by Olga Vinogradova and Jun Qin The Use of Residual Dipolar Coupling in Studying Proteins by NMR, by Kang Chen und Nico Tjandra NMR Studies of Metalloproteins, by Hongyan Li and Hongzhe Sun Recent Developments in 15N NMR Relaxation Studies that Probe Protein Backbone Dynamics, by Rieko Ishima Contemporary Methods in Structure Determination of Membrane Proteins by Solution NMR, by Tabussom Qureshi and Natalie K. Goto Protein Structure Determination by Solid-State NMR, by Xin Zhao Dynamic Nuclear Polarization: New Methodology and Applications, by Kong Hung Sze, Qinglin Wu, Ho Sum Tse and Guang Zhu
Download or read book Solid state NMR Structural Studies of Proteins Using Cyclen Based Paramagnetic Metal Chelating Probes written by Rajith Madushanka Jayasinha Arachchige and published by . This book was released on 2016 with total page pages. Available in PDF, EPUB and Kindle. Book excerpt: The capability of solid-state NMR spectroscopy to provide site-specific atomic-level information makes it one of the main tools used in the structural and dynamic analysis of complex non-crystalline biological macromolecules. However, the challenges associated with measurements of unambiguous long-range distance restraints between nuclear spins by conventional solid-state NMR methods have a significant impact on the ability to determine three-dimensional structures of proteins and nucleic acids. Recently, it has been shown that paramagnetism-based solid-state NMR methods can be utilized to overcome this scarcity of long-range structural information. Electron-nucleus through space dipolar interactions in proteins containing paramagnetic metal centers lead to NMR spectral effects including paramagnetic relaxation enhancements (PREs) and pseudocontact shifts (PCSs), which can provide structural restraints up to 30 A° and beyond exceeding by four to five-fold the length scales accessible by conventional methods. For natively diamagnetic proteins with no endogenous paramagnetic metal centers can be introduced by covalently linking to the protein small molecule tags containing high affinity metal binding motifs. The focus of this research was to develop new thiol-reactive mono and bidentate compact paramagnetic metal chelating probes based on the cyclen manifold for improved solid-state NMR PRE and PCS measurements in natively diamagnetic proteins. The single arm TETAC tag was able to overcome the key shortcomings associated with the more bulky and flexible EDTA type metal-binding tags used in initial paramagnetic solid-state NMR studies. Relative to PREs, the magnitude of which depends primarily on the electron-nucleus distance, the measurements of PCS effects are far more challenging due to an additional dependence on the location of the nucleus in the frame of the g-tensor of the unpaired electron spin of the paramagnetic center. Specifically, such measurements are susceptible to the flexibility of the paramagnetic tag, which can considerably reduce the PCS magnitude or average the effect altogether. To alleviate this problem compact cyclen based tags, which can rigidly be attached to the protein via two disulfide bridges, were designed. The new double arm tags, 2,2'-(1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(N-(2-(pyridin-2-yldisulfanyl)ethyl)acetamide) and 2,2'-(4,10-bis(2-(pyridin-2-yldisulfanyl)ethyl)-1,4,7,10-tetraazacyclododecane-1,7-diyl)diacetic acid, are able to immobilize paramagnetic Co(II) ions on the model 56 amino acid residue protein, B1 immunoglobulin-binding domain of protein G, and successfully overcome the PCS averaging issues associated with the monodentate metal chelating probes. In addition, the same tags loaded with Cu(II) enable solid-state NMR PRE measurements to be performed to yield additional restraints on the protein structure.
Download or read book Mas Solid State Nmr on Biomolecules written by Rasmus Linser and published by Sudwestdeutscher Verlag Fur Hochschulschriften AG. This book was released on 2011 with total page 192 pages. Available in PDF, EPUB and Kindle. Book excerpt: Due to numerous achievements in the last years, solid-state NMR has evolved a potent tool for structural characterization of biomolecules. Not relying on single crystals or solubility, the technique particularly focuses on fibrillar and membrane proteins, which are difficult to characterize otherwise. Despite this enormous potential, numerous difficulties unsolved to date demand for further technical and methodological reworking. Among these, the achievable signal to noise and resolution are the most prominent limits. Whereas a series of limitations is induced by strong dipolar interactions among protons even under fast MAS (Magic Angle Spinning), a (partial) dilution of the proton content by deuterons bears a number of spectroscopic advantages. These are e.g. direct 1H detection with an excellent resolution, accessibility of long-range distance restraints, and proton based dynamics and surface accessibility determination. Besides, relaxation for various coherences is significantly decreased, making solution-NMR like multi-dimensional experiments for peak assignment etc. possible. The features of a dilute protonation explored in this work have lead to 12 peer-reviewed publications.
Download or read book Solution NMR of Paramagnetic Molecules written by Ivano Bertini and published by Elsevier. This book was released on 2001-07-04 with total page 392 pages. Available in PDF, EPUB and Kindle. Book excerpt: NMR is a growing technique which represents a generalized, spread, common tool for spectroscopy and for structural and dynamic investigation. Part of the field of competence of NMR is represented by molecules with unpaired electrons, which are called paramagnetic. The presence of unpaired electrons is at the same time a drawback (negative effect) and a precious source of information about structure and dynamics. New phenomena and effects are described which are due to the high magnetic fields and advances in the methodology. Solution NMR of Paramagnetic Molecules is unique in dealing with these matters. The scope is that of presenting a complete description, which is both rigorous and pictorial, of theory and experiments of NMR of paramagnetic molecules in solution. Pertinent examples are described. From the time dependent behaviour of electrons in the various metal ions including polimetallic systems to the hyperfine-based information, and from NMR experiments to constraints for solution structure determination. The book's major theme is how to perform high resolution NMR experiments and how to obtain structural and dynamic information on paramagnetic metal ion containing systems.
Download or read book Multidimensional Solid State NMR and Polymers written by Klaus Schmidt-Rohr and published by Elsevier. This book was released on 2012-12-02 with total page 501 pages. Available in PDF, EPUB and Kindle. Book excerpt: NMR spectroscopy is the most valuable and versatile analytical tool in chemistry. While excellent monographs exist on high-resolution NMR in liquids and solids, this is the first book to address multidimensional solid-state NMR. Multidimensional techniques enable researchers to obtain detailed information about the structure, dynamics, orientation, and phase separation of solids, which provides the basis of a better understanding of materials properties on the molecular level.Dramatic progress-much of it pioneered by the authors-has been achieved in this area, especially in synthetic polymers. Solid-state NMR now favorably competes with well-established techniques, such as light, x-ray, or neutron scattering, electron microscopy, and dielectric and mechanical relaxation.The application of multidimensional solid-state NMR inevitably involves use of concepts from different fields of science. This book also provides the first comprehensive treatment of both the new experimental techniques and the theoretical concepts needed in more complex data analysis. The text addresses spectroscopists and polymer scientists by treating the subject on different levels; descriptive, technical, and mathematical approaches are used when appropriate. It presents an overview of new developments with numerous experimental examples and illustrations, which will appeal to readers interested in both the information content as well as the potential of solid-state NMR. The book also contains many previously unpublished details that will be appreciated by those who want to perform the experiments. The techniques described are applicable not only to the study of synthetic polymers but to numerous problems in solid-state physics, chemistry, materials science, and biophysics. Presents original theories and new perspectives on scattering techniques Provides a systematic treatment of the whole subject Gives readers access to previously unpublished material Includes extensive illustrations
Download or read book Experimental Approaches of NMR Spectroscopy written by The Nuclear Magnetic Resonance Society of Japan and published by Springer. This book was released on 2017-11-23 with total page 634 pages. Available in PDF, EPUB and Kindle. Book excerpt: This book describes the advanced developments in methodology and applications of NMR spectroscopy to life science and materials science. Experts who are leaders in the development of new methods and applications of life and material sciences have contributed an exciting range of topics that cover recent advances in structural determination of biological and material molecules, dynamic aspects of biological and material molecules, and development of novel NMR techniques, including resolution and sensitivity enhancement. First, this book particularly emphasizes the experimental details for new researchers to use NMR spectroscopy and pick up the potentials of NMR spectroscopy. Second, the book is designed for those who are involved in either developing the technique or expanding the NMR application fields by applying them to specific samples. Third, the Nuclear Magnetic Resonance Society of Japan has organized this book not only for NMR members of Japan but also for readers worldwide who are interested in using NMR spectroscopy extensively.
Download or read book Development of New Paramagnetic Tags for Solid state NMR Structural Studies of Natively Diamagnetic Proteins written by Jayasimha Arachchige and published by . This book was released on 2014 with total page pages. Available in PDF, EPUB and Kindle. Book excerpt: Solid state NMR is a powerful technique, which can be used for structural and dynamic studies of complex biological macromolecules. However, the paucity of structural restraints available using conventional techniques complicates the structural studies of proteins by solid-state NMR. Recently, it has been shown that large numbers of long range distance restraints in the form of paramagnetic relaxation enhancements (PREs) and pseudocontact shifts (PCS) can be derived from proteins containing paramagnetic centers.
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.-
