Protein NMR Spectroscopy (PDF)

List of Contributors xiii Introduction 1 Lu-Yun Lian and Gordon Roberts References 4 1 Sample Preparation, Data Collection and Processing 5 Frederick W. Muskett 1.1 Introduction 5 1.2 Sample Preparation 5 1.3 Data Collection 11 1.4 Data Processing 17 2 Isotope Labelling 23 Mitsuhiro Takeda and Masatsune Kainosho 2.1 Introduction 23 2.2 Production Methods for Isotopically Labelled Proteins 24 2.3 Uniform Isotope Labelling of Proteins 29 2.4 Selective Isotope Labelling of Proteins 32 2.5 Segmental Labelling 37 2.6 SAIL Methods 38 2.7 Concluding Remarks 45 3 Resonance Assignments 55 Lu-Yun Lian and Igor L. Barsukov 3.1 Introduction 55 3.2 Resonance Assignment of Unlabelled Proteins 56 3.3 15N-Edited Experiments 60 3.4 Triple Resonance 62 3.5 Side-Chain Assignments 77 4 Measurement of Structural Restraints 83 Geerten W. Vuister, Nico Tjandra, Yang Shen, Alex Grishaev and Stephan Grzesiek 4.1 Introduction 83 4.2 NOE-Based Distance Restraints 84 4.3 Dihedral Restraints Derived from J-Couplings 96 4.4 Hydrogen Bond Restraints 103 4.5 Orientational Restraints 107 4.6 Chemical Shift Structural Restraints 129 4.7 Solution Scattering Restraints 137 5 Calculation of Structures from NMR Restraints 159 Peter Guntert 5.1 Introduction 159 5.2 Historical Development 161 5.3 Structure Calculation Algorithms 164 5.4 Automated NOE Assignment 173 5.5 Nonclassical Approaches 178 5.6 Fully Automated Structure Analysis 181 6 Paramagnetic Tools in Protein NMR 193 Peter H.J. Keizers and Marcellus Ubbink 6.1 Introduction 193 6.2 Types of Restraints 194 6.3 What Metals to Use? 200 6.4 Paramagnetic Probes 203 6.5 Examples 209 6.6 Conclusions and Perspective 212 7 Structural and Dynamic Information on Ligand Binding 221 Gordon Roberts 7.1 Introduction 221 7.2 Fundamentals of Exchange Effects on NMR Spectra 222 7.3 Measurement of Equilibrium and Rate Constants 229 7.4 Detecting Binding - NMR Screening 238 7.5 Mechanistic Information 241 7.6 Structural Information 246 8 Macromolecular Complexes

Professor Gordon Roberts is Head of the School of Biological Sciences, University of Leicester.

Dr Christina Redfield is Reader, Oxford Centre for Molecular Sciences, University of Oxford.

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