Two-Dimensional (2D) NMR Methods

K.L. Ivanov (International Tomography Center, Novosibirsk, Russia) was actively involved in teaching at the Novosibirsk State University, ITC Novosibirsk, and at various schools for young researchers, and was a specialist in NMR theory and NMR methods development, notably, spin hyperpolarization methods.P.K. Madhu (Tata Institute of Fundamental Research, Hyderabad, India) has contributed to NMR relaxation theory, methods development in solid-state NMR and biophysical applications of NMR. He currently has interests in zero-field NMR and application of NMR in perovskites and battery materials.G. Rajalakshmi (Tata Institute of Fundamental Research, Hyderabad, India) is an experimental physicist developing zero to ultra-low field NMR techniques for solid-state experiments. She also works on nonlinear optical-atomic magnetometry methods for detecting dc to rf magnetic fields.

• Dedication vList of Contributors xviiPreface xix1 Basics of Two-dimensional NMR 1Malcolm H. Levitt1.1 Introduction 11.2 Spin Dynamics 21.3 One-dimensional Fourier NMR 61.4 Two-dimensional NMR 111.5 Summary 142 Data Processing Methods: Fourier and Beyond 19Vladislav Orekhov, Pawel Kasprzak, and Krzysztof Kazimierczuk2.1 Introduction 192.2 Time-domain NMR Signal 192.3 NMR Spectrum 202.4 The Most Important Features of FT 202.5 Distortion: Phase 232.6 Kramers-Kronig Relations and Hilbert Transform 232.7 Distortion: Truncation 252.8 Distortion: Noise and Multiple Scans 272.9 Distortion: Sampling and DFT 272.10 Quadrature Detection 302.11 Processing:Weighting 312.12 Processing: Zero Filling 332.13 Fourier Transform in Multiple Dimensions 332.14 Quadrature Detection in Multiple Dimensions 362.15 Projection Theorem 372.16 ND Sampling Aspects and Sparse Sampling 402.17 Reconstructing Sparsely Sampled Data Sets 412.18 Deconvolution 423 Product Operator Formalism 47Rolf Boelens and Robert Kaptein3.1 Introduction 473.2 Product Operators and Time Evolution 483.3 Time Evolution of the Product Operators 553.4 Applications 593.4.1 Spin-echo Experiments 593.5 Two-dimensional Experiments 664 Relaxation in NMR Spectroscopy 93Matthias Ernst4.1 Introduction 934.2 Theory 954.3 Relaxation in Spin-1/2 Systems: Dipolar and CSA Relaxation 1044.4 Other Relaxation Mechanisms 1254.5 Concluding Remarks 1305 Coherence Transfer Pathways 135David E. Korenchan and Alexej Jerschow5.1 Coherence Transfer Pathways: What and Why? 1355.2 Principles of Coherence Selection 1375.3 Coherence Transfer Pathway Selection by Phase Cycling 1405.4 Cogwheel Phase Cycling 1465.5 Coherence Transfer Pathway Selection by Pulsed-field Gradients 1475.6 Comparison Between Phase Cycling and Pulsed-field Gradients 1505.7 CTP Selection in Heteronuclear Spin Systems 1505.8 Additional Approaches to Coherence Selection 1516 Nuclear Overhauser Effect Spectroscopy 153P.K. Madhu6.1 Introduction 1536.2 Nuclear Overhauser Effect 1536.3 Measurement of NOE 1616.4 Heteronuclear NOE 1616.5 NOE Kinetics 1626.6 Nuclear Overhauser Effect Spectroscopy, NOESY 1646.7 Rotating-frame NOE, ROE 1666.8 Relative Signs of Cross Peaks 1686.9 Generalised Solomon’s Equation 1696.10 NOESY and ROESY: Practical Considerations and Experimental Spectra 1706.11 Conclusions 1707 DOSY Methods for Studying Non-equilibrium Molecular and Ionic Systems 175Muslim Dvoyashkin, Monika Schoönhoff, and Ville-Veikko Telkki7.1 Introduction 1757.2 Spatial Spin "Encoding" Using Magnetic Field Gradient 1757.3 Formation of NMR Signal and Spin Echo in the Presence of Field Gradient 1767.4 NMR of Liquids in An Electric Field: Electrophoretic NMR 1787.5 Ultrafast Diffusion Measurements 1867.6 Ultrafast Diffusion Exchange Spectroscopy 1898 Multiple Acquisition Strategies 195Nathaniel J. Traaseth8.1 Introduction 1958.2 Types of Multiple Acquisition Experiments 1958.3 Utilization of Forgotten Spin Operators 1968.4 Application of Multiple Acquisition Techniques 1988.5 Modularity of Multiple Detection Schemes and Other Novel Approaches 2018.6 Future of Multiple Acquisition Detection 2029 Anisotropic One-dimensional/Two-dimensional NMR in Molecular Analysis 209Philippe Lesot and Roberto R. Gil9.1 Introduction 2099.2 Advantages of Oriented Solvents 2109.3 Description of Useful Anisotropic NMR Parameters 2139.4 Adapted 2D NMR Tools 2219.5 Examples of Polymeric Liquid Crystals 2269.6 Contribution to the Analysis of Chiral and Prochiral Molecules 2329.7 Structural Value of Anisotropic NMR Parameters 2489.8 Conformational Analysis in Oriented Solvents 2769.9 Anisotropic 2H 2D NMR Applied to Molecular Isotope Analysis 2779.10 Anisotropic NMR in Molecular Analysis: What You Should Keep in Mind 28110 Ultrafast 2D methods 297Boris Gouilleux10.1 Introduction 29710.2 UF 2D NMR Principles: Entangling the Space and the Time 29910.3 Specific Features of UF 2D NMR 30510.4 Advanced UF Methods 30710.5 UF 2D NMR: A Versatile Approach 31110.6 Overview of UF 2D NMR Applications 31610.7 Conclusion 32611 Multi-dimensional Methods in Biological NMR 333Tobias Schneider and Michael Kovermann11.1 Introduction 33311.2 Experimental Approaches 33411.3 Case Studies 33812 TROSY: Principles and Applications 365Harindranath Kadavath and Roland Riek12.1 Introduction 36512.2 The Principles of TROSY 36612.3 Practical Aspects of TROSY 37112.4 Applications of TROSY 37412.5 Transverse Relaxation-optimization in the Polarization Transfers 37912.6 15N Direct Detected TROSY 38012.7 [1H,13C]-TROSY Correlation Experiments 38012.8 Applications to Nucleic Acids 38212.9 Intermolecular Interactions and Drug Design 38312.10 Conclusion 38313 Two-Dimensional Methods and Zero- to Ultralow-Field (ZULF) NMR 395K.L. Ivanov, John Blanchard, Dmitry Budker, Fabien Ferrage, Alexey Kiryutin, Tobias Sjolander, Alexandra Yurkovskaya, and Ivan Zhukov13.1 Introduction and Motivation 39513.2 EarlyWork 39613.3 Two-dimensional NMR Measured at Zero Magnetic Field 39713.4 Nuclear Magnetic Resonance at Millitesla Fields Using a Zero-Field Spectrometer 40313.5 Field Cycling NMR and Correlation Spectroscopy 40413.6 ZERO-Field - High-Field Comparison 40913.7 Conclusion and Outlook 41214 Multidimensional Methods and Paramagnetic NMR 415Thomas Robinson, Kevin J. Sanders, Andrew J. Pell, and Guido Pintacuda14.1 Introduction 41514.2 NMR Methods for Paramagnetic Systems in Solution 41614.3 NMR Methods for Paramagnetic Systems in Solids 42315 Chemical Exchange 435Ashok Sekhar and Pramodh Vallurupalli15.1 Introduction 43515.2 Bloch-McConnell Equations 43615.3 Studying Exchange Between Visible States 44315.4 Studying Exchange Between a Visible State and Invisible State(s) 44815.5 Summary 458Acknowledgments 459References 459Appendix A Proton-Detected Heteronuclear and Multidimensional NMR 461Christian Griesinger, Harald Schwalbe, Jürgen Schleucher, and Michael SattlerIndex 553