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From complex structure elucidation to biomolecular interactions - this applicationoriented textbook covers both theory and practice of modern NMR applications. Part one sets the stage with a general description of NMR introducing important parameters such as the chemical shift and scalar or dipolar couplings. Part two describes the theory behind NMR, providing a profound understanding of the involved spin physics, deliberately kept shorter than in other NMR textbooks, and without a rigorous mathematical treatment of all the physico-chemical computations. Part three discusses technical and…mehr
From complex structure elucidation to biomolecular interactions - this applicationoriented textbook covers both theory and practice of modern NMR applications. Part one sets the stage with a general description of NMR introducing important parameters such as the chemical shift and scalar or dipolar couplings. Part two describes the theory behind NMR, providing a profound understanding of the involved spin physics, deliberately kept shorter than in other NMR textbooks, and without a rigorous mathematical treatment of all the physico-chemical computations. Part three discusses technical and practical aspects of how to use NMR. Important phenomena such as relaxation, exchange, or the nuclear Overhauser effects and the methods of modern NMR spectroscopy including multidimensional experiments, solid state NMR, and the measurement of molecular interactions are the subject of part four. The final part explains the use of NMR for the structure determination of selected classes of complex biomolecules, from steroids to peptides or proteins, nucleic acids, and carbohydrates. For chemists as well as users of NMR technology in the biological sciences.
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Autorenporträt
Oliver Zerbe is the head of the NMR department at the University of Zurich. He studied chemistry and obtained his PhD under the supervision of Wolfgang von Philipsborn in Zurich. After a postdoctoral stay in the group of Kurt Wüthrich at the ETH Zurich he conducted his habilitation with Gerd Folkers at the Institute of Pharmaceutical Sciences at the ETH. In 2003 he returned to his present location at the University of Zurich, where he is now a professor in the Department of Chemistry. His main interests are structures of proteins, particularly of membrane proteins. Oliver Zerbe is the author of approximately 100 scientific publications in peer-reviewed journals and has edited one book, "NMR in drug research". After studying chemistry at the University of Applied Sciences of Bern, Simon Jurt has been working for more than ten years in the NMR department of the University of Zurich. In addition to maintenance and trouble shooting of the NMR spectrometers, he introduces the students to the secrets of NMR spectroscopy, teaches practical NMR courses and is involved in several research projects. His main interests are the experimental NMR techniques, which allow obtaining a plethora of chemo-physical information from the spin physics.
Inhaltsangabe
Preface INTRODUCTION TO NMR SPECTROSCOPY Our First 1D Spectrum Some Nomenclature: Chemical Shifts, Line Widths, and Scalar Couplings Interpretation of Spectra: A Simple Example Two-Dimensional NMR Spectroscopy: An Introduction PART ONE - Basics of Solution NMR BASICS OF 1D NMR SPECTROSCOPY The Principles of NMR Spectroscopy The Chemical Shift Scalar Couplings Relaxation and the Nuclear Overhauser Effect Practical Aspects Problems 1H NMR General Aspects Chemical Shifts Spin Systems, Symmetry, and Chemical or Magnetic Equivalence Scalar Coupling 1H-1H Coupling Constants Problems NMR OF 13C AND HETERONUCLEI Properties of Heteronuclei Indirect Detection of Spin-1/2 Nuclei 13C NMR Spectroscopy NMR of Other Main Group Elements NMR Experiments with Transition Metal Nuclei Problems PART TWO - Theory of NMR Spectroscopy NUCLEAR MAGNETISM - A MICROSCOPIC VIEW The Origin of Magnetism Spin - An Intrinsic Property of Many Particles Experimental Evidence for the Quantization of the Dipole Moment: The Stern-Gerlach Experiment The Nuclear Spin and Its Magnetic Dipole Moment Nuclear Dipole Moments in a Homogeneous Magnetic Field: The Zeeman Effect Problems MAGNETIZATION - A MACROSCOPIC VIEW The Macroscopic Magnetization Magnetization at Thermal Equilibrium Transverse Magnetization and Coherences Time Evolution of Magnetization The Rotating Frame of Reference RF Pulses Problems CHEMICAL SHIFT AND SCALAR AND DIPOLAR COUPLINGS Chemical Shielding The Spin-Spin Coupling Problems A FORMAL DESCRIPTION OF NMR EXPERIMENTS: THE PRODUCT OPERATOR FORMALISM Description of Events by Product Operators Classification of Spin Terms Used in the POF Coherence Transfer Steps An Example Calculation for a Simple 1D Experiment A BRIEF INTRODUCTION INTO THE QUANTUM-MECHANICAL CONCEPT OF NMR Wave Functions, Operators, and Probabilities Mathematical Tools in the Quantum Description of NMR The Spin Space of Single Noninteracting Spins Hamiltonian and Time Evolution Free Precession Representation of Spin Ensembles - The Density Matrix Formalism Spin Systems PART THREE - Technical Aspects of NMR THE COMPONENTS OF AN NMR SPECTROMETER The Magnet Shim Systems and Shimming The Electronics The Probehead The Lock System Problems ACQUISITION AND PROCESSING The Time Domain Signal Fourier Transform Technical Details of Data Acquisition Data Processing Problems EXPERIMENTAL TECHNIQUES RF Pulses Pulsed Field Gradients Phase Cycling Decoupling Isotropic Mixing Solvent Suppression Basic 1D Experiments Measuring Relaxation Times The INEPT Experiment The DEPT Experiment Problems THE ART OF PULSE EXPERIMENTS Introduction Our Toolbox: Pulses, Delays, and Pulsed Field Gradients The Excitation Block The Mixing Period Simple Homonuclear 2D Sequences Heteronuclear 2D Correlation Experiments Experiments for Measuring Relaxation Times Triple-Resonance NMR Experiments Experimental Details Problems PART FOUR - Important Phenomena and Methods in Modern NMR RELAXATION Introduction Relaxation: The Macroscopic Picture The Microscopic Picture: Relaxation Mechanisms Relaxation and Motion Measuring 15N Relaxation to Determine Protein Dynamics Measurement of Relaxation Dispersion Problems THE NUCLEAR OVERHAUSER EFFECT Introduction The Formal Description of the NOE: The Solomon Equations Applications of the NOE in Stereochemical Analysis Practical Tips for Measuring NOEs Problems CHEMICAL AND CONFORMATIONAL EXCHANGE Two-Site Exchange Experimental Determination of the Rate Constants Determination of the Activation Energy by Variable-Temperature NMR Experiments Problems TWO-DIMENSIONAL NMR SPECTROSCOPY Introduction The Appearance of 2D Spectra Two-Dimensional NMR Spectroscopy: How Does It Work? Types of 2D NMR Experiments Three-Dimensional NMR Spectroscopy Practical Aspects of Measuring 2D Spectra Problems SOLID-STATE NMR EXPERIMENTS Introduction The Chemical Shift in the Solid State Dipolar Couplings in the Solid State Removing CSA and Dipolar Couplings: Magic-Angle Spinning Reintroducing Dipolar Couplings under MAS Conditions Polarization Transfer in the Solid State: Cross-Polarization Technical Aspects of Solid-State NMR Experiments Problems DETECTION OF INTERMOLECULAR INTERACTIONS Introduction Chemical Shift Perturbation Methods Based on Changes in Transverse Relaxation (Ligand-Observe Methods) Methods Based on Changes in Cross-Relaxation (NOEs) (Ligand-Observe or Target-Observe Methods) Methods Based on Changes in Diffusion Rates (Ligand-Observe Methods) Comparison of Methods Problems PART FIVE - Structure Determination of Natural Products by NMR CARBOHYDRATES The Chemical Nature of Carbohydrates NMR Spectroscopy of Carbohydrates Quick Identification A Worked Example: Sucrose STEROIDS Introduction A Worked Example: Prednisone PEPTIDES AND PROTEINS Introduction The Structure of Peptides and Proteins NMR of Peptides and Proteins Assignment of Peptide and Protein Resonances A Worked Example: The Pentapeptide TP5 NUCLEIC ACIDS Introduction The Structure of DNA and RNA NMR of DNA and RNA Assignment of DNA and RNA Resonances APPENDIX The Magnetic H and B Fields Magnetic Dipole Moment and Magnetization Scalars, Vectors, and Tensors Properties of Matrices
Preface INTRODUCTION TO NMR SPECTROSCOPY Our First 1D Spectrum Some Nomenclature: Chemical Shifts, Line Widths, and Scalar Couplings Interpretation of Spectra: A Simple Example Two-Dimensional NMR Spectroscopy: An Introduction PART ONE - Basics of Solution NMR BASICS OF 1D NMR SPECTROSCOPY The Principles of NMR Spectroscopy The Chemical Shift Scalar Couplings Relaxation and the Nuclear Overhauser Effect Practical Aspects Problems 1H NMR General Aspects Chemical Shifts Spin Systems, Symmetry, and Chemical or Magnetic Equivalence Scalar Coupling 1H-1H Coupling Constants Problems NMR OF 13C AND HETERONUCLEI Properties of Heteronuclei Indirect Detection of Spin-1/2 Nuclei 13C NMR Spectroscopy NMR of Other Main Group Elements NMR Experiments with Transition Metal Nuclei Problems PART TWO - Theory of NMR Spectroscopy NUCLEAR MAGNETISM - A MICROSCOPIC VIEW The Origin of Magnetism Spin - An Intrinsic Property of Many Particles Experimental Evidence for the Quantization of the Dipole Moment: The Stern-Gerlach Experiment The Nuclear Spin and Its Magnetic Dipole Moment Nuclear Dipole Moments in a Homogeneous Magnetic Field: The Zeeman Effect Problems MAGNETIZATION - A MACROSCOPIC VIEW The Macroscopic Magnetization Magnetization at Thermal Equilibrium Transverse Magnetization and Coherences Time Evolution of Magnetization The Rotating Frame of Reference RF Pulses Problems CHEMICAL SHIFT AND SCALAR AND DIPOLAR COUPLINGS Chemical Shielding The Spin-Spin Coupling Problems A FORMAL DESCRIPTION OF NMR EXPERIMENTS: THE PRODUCT OPERATOR FORMALISM Description of Events by Product Operators Classification of Spin Terms Used in the POF Coherence Transfer Steps An Example Calculation for a Simple 1D Experiment A BRIEF INTRODUCTION INTO THE QUANTUM-MECHANICAL CONCEPT OF NMR Wave Functions, Operators, and Probabilities Mathematical Tools in the Quantum Description of NMR The Spin Space of Single Noninteracting Spins Hamiltonian and Time Evolution Free Precession Representation of Spin Ensembles - The Density Matrix Formalism Spin Systems PART THREE - Technical Aspects of NMR THE COMPONENTS OF AN NMR SPECTROMETER The Magnet Shim Systems and Shimming The Electronics The Probehead The Lock System Problems ACQUISITION AND PROCESSING The Time Domain Signal Fourier Transform Technical Details of Data Acquisition Data Processing Problems EXPERIMENTAL TECHNIQUES RF Pulses Pulsed Field Gradients Phase Cycling Decoupling Isotropic Mixing Solvent Suppression Basic 1D Experiments Measuring Relaxation Times The INEPT Experiment The DEPT Experiment Problems THE ART OF PULSE EXPERIMENTS Introduction Our Toolbox: Pulses, Delays, and Pulsed Field Gradients The Excitation Block The Mixing Period Simple Homonuclear 2D Sequences Heteronuclear 2D Correlation Experiments Experiments for Measuring Relaxation Times Triple-Resonance NMR Experiments Experimental Details Problems PART FOUR - Important Phenomena and Methods in Modern NMR RELAXATION Introduction Relaxation: The Macroscopic Picture The Microscopic Picture: Relaxation Mechanisms Relaxation and Motion Measuring 15N Relaxation to Determine Protein Dynamics Measurement of Relaxation Dispersion Problems THE NUCLEAR OVERHAUSER EFFECT Introduction The Formal Description of the NOE: The Solomon Equations Applications of the NOE in Stereochemical Analysis Practical Tips for Measuring NOEs Problems CHEMICAL AND CONFORMATIONAL EXCHANGE Two-Site Exchange Experimental Determination of the Rate Constants Determination of the Activation Energy by Variable-Temperature NMR Experiments Problems TWO-DIMENSIONAL NMR SPECTROSCOPY Introduction The Appearance of 2D Spectra Two-Dimensional NMR Spectroscopy: How Does It Work? Types of 2D NMR Experiments Three-Dimensional NMR Spectroscopy Practical Aspects of Measuring 2D Spectra Problems SOLID-STATE NMR EXPERIMENTS Introduction The Chemical Shift in the Solid State Dipolar Couplings in the Solid State Removing CSA and Dipolar Couplings: Magic-Angle Spinning Reintroducing Dipolar Couplings under MAS Conditions Polarization Transfer in the Solid State: Cross-Polarization Technical Aspects of Solid-State NMR Experiments Problems DETECTION OF INTERMOLECULAR INTERACTIONS Introduction Chemical Shift Perturbation Methods Based on Changes in Transverse Relaxation (Ligand-Observe Methods) Methods Based on Changes in Cross-Relaxation (NOEs) (Ligand-Observe or Target-Observe Methods) Methods Based on Changes in Diffusion Rates (Ligand-Observe Methods) Comparison of Methods Problems PART FIVE - Structure Determination of Natural Products by NMR CARBOHYDRATES The Chemical Nature of Carbohydrates NMR Spectroscopy of Carbohydrates Quick Identification A Worked Example: Sucrose STEROIDS Introduction A Worked Example: Prednisone PEPTIDES AND PROTEINS Introduction The Structure of Peptides and Proteins NMR of Peptides and Proteins Assignment of Peptide and Protein Resonances A Worked Example: The Pentapeptide TP5 NUCLEIC ACIDS Introduction The Structure of DNA and RNA NMR of DNA and RNA Assignment of DNA and RNA Resonances APPENDIX The Magnetic H and B Fields Magnetic Dipole Moment and Magnetization Scalars, Vectors, and Tensors Properties of Matrices
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