A Complete Introduction to MODERN NMR Spectroscopy, Written by Roger S. Macomber
Free Download A Complete Introduction to MODERN NMR Spectroscopy by Roger S. Macomber
A Complete Introduction to MODERN NMR Spectroscopy
Author
Roger S. Macomber
CONTENTS
Preface xi
Acknowledgments xiii
Frequently Used Symbols and Abbreviations xv
Chapter 1 SPECTROSCOPY: SOME PRELIMINARY CONSIDERATIONS
J . 1 What is NMR Spectroscopy? 1 .2 Properties of Electromagnetic Radiation 1 .3 Interaction of Radiation with Matter: The Classical Picture 1 .4 Uncertainty and the Question of Time Scale Chapter Summary Review Problems
Chapter 2 MAGNETIC PROPERTIES OF NUCLEI
2.1 The Structure of an Atom 2.2 The Nucleus in a Magnetic Field 2.3 Nuclear Energy Levels and Relaxation Times 2.4 The Rotating Frame of Reference 2.5 Relaxation Mechanisms and Correlation Times Chapter Summary Additional Resources Review Problems
Chapter 3 OBTAINING AN NMR SPECTRUM
3.1 Electricity and Magnetism 3.2 The NMR Magnet 3.3 Signal Generation the Old Way: The Continuous-Wave (CW) Experiment 3.4 The Modern Pulsed Mode for Signal Acquisition 3.5 Line Widths, Lineshape, and Sampling Considerations 3.6 Measurement of Relaxation Times Chapter Summary Additional Resources Review Problems
Chapter 4 A LITTLE BIT OF SYMMETRY
4.1 Symmetry Operations and Distinguishability 4.2 Conformations and Their Symmetry 4.3 Homotopic, Enantiotopic, and Diastereotopic Nuclei 4.4 Accidental Equivalence Chapter Summary Additional Resources Review Problems
Chapter 5 THE H AND 13 C NMR SPECTRA OF TOLUENE
5.1 The ‘H NMR Spectrum of Toluene at 80 MHz 5.2 The Chemical Shift Scale 5.3 The 250- and 400-MHz ‘H NMR Spectra of Toluene 5.4 The 1 3 C NMR Spectrum of Toluene at 20. 1, 62.9, and 1 00.6 MHz 5.5 Data Acquisition Parameters Chapter Summary Review Problems
Chapter 6 CORRELATING PROTON CHEMICAL SHIFTS WITH MOLECULAR STRUCTURE
6.1 Shielding and Deshielding 6.2 Chemical Shifts of Hydrogens Attached to Tetrahedral Carbon 6.3 Vinyl and Formyl Hydrogen Chemical Shifts 6.4 Magnetic Anisotropy 6.5 Aromatic Hydrogen Chemical Shift Correlations 6.6 Hydrogen Attached to Elements Other than Carbon Chapter Summary References Additional Resources Review Problems
Chapter 7 CHEMICAL SHIFT CORRELATIONS FOR 13 C AND OTHER ELEMENTS
7.1 l3 C Chemical Shifts Revisited 7.2 Tetrahedral (sp 2 Hybridized) Carbons 7.3 Heterocyclic Structures 7.4 Trigonal Carbons 7.5 Triple Bonded Carbons 7.6 Carbonyl Carbons 7.7 Miscellaneous Unsaturated Carbons 7.8 Summary of l3 C Chemical Shifts 7.9 Chemical Shifts of Other Elements Chapter Summary References Review Problems
SELF-TEST I
Chapter 8 FIRST-ORDER (WEAK) SPIN-SPIN COUPLING
8.1 Unexpected Lines in an NMR Spectrum 8.2 The ‘H Spectrum of Diethyl Ether 8.3 Homonuclear ‘H Coupling: The Simplified Picture 8.4 The Spin-Spin Coupling Checklist 8.5 Thew+lRule 8.6 Heteronuclear Spin-Spin Coupling 8.7 Review Examples Chapter Summary Review Problems
Chapter 9 FACTORS THAT INFLUENCE THE SIGN AND MAGNITUDE OF SECOND-ORDER (STRONG) COUPLING EFFECTS
9.1 Nuclear Spin Energy Diagrams and the Sign of J 9.2 Factors that Influence /: Preliminary Considerations 9.3 One-Bond Coupling Constants 9.4 Two-Bond (Geminal) Coupling Constants 9.5 Three-Bond (Vicinal) Coupling Constants 9.6 Long-Range Coupling Constants 9.7 Magnetic Equivalence 9.8 Pople Spin System Notation 9.9 Slanting Multiplets and Second-Order (Strong Coupling) Effects 9.10 Calculated Spectra 9.11 The AX -> AB -> A 2 Continuum 9.12 More About the ABX System: Deceptive Simplicity and Virtual Coupling Chapter Summary References Review Problems
Chapter 10 THE STUDY OF DYNAMIC PROCESSES BY NMR
10.1 Reversible and Irreversible Dynamic Processes 10.2 Reversible Intramolecular Processes Involving Rotation Around Bonds 10.3 Simple Two-Site Intramolecular Exchange 10.4 Reversible Intramolecular Chemical Processes 10.5 Reversible Intermolecular Chemical Processes 10.6 Reversible Intermolecular Complexation 1 0.7 Other Examples of Reversible Complexation: Chemical Shift Reagents Chapter Summary References Review Problems
Chapter 11 ELECTRON PARAMAGNETIC RESONANCE SPECTROSCOPY AND CHEMICALLY INDUCED DYNAMIC NUCLEAR POLARIZATION
11.1 Electron Paramagnetic Resonance 11.2 Free Radicals 11.3 The £ Factor 11 .4 Sensitivity Considerations 11 .5 Hyperfine Coupling and the a Value 11.6 A Typical EPR Spectrum 11 .7 CIDNP: Mysterious Behavior of NMR Spectrometers 11.8 The Net Effect 11.9 The Multiple! Effect 11.10 The Radical-Pair Theory of The Net Effect 11.11 The Radical-Pair Theory of the Multiplet Effect 11.12 A Few Final Words about CIDNP Chapter Summary References Review Problems
Chapter 12 DOUBLE-RESONANCE TECHNIQUES AND COMPLEX PULSE SEQUENCES
12.1 What is Double Resonance? 12.2 Heteronuclear Spin Decoupling 12.3 Polarization Transfer and the Nuclear Overhauser Effect 12.4 Gated and Inverse Gated Decoupling 12.5 Off-Resonance Decoupling 12.6 Homonuclear Spin Decoupling 12.7 Homonuclear Difference NOE: The Test for Proximity 12.8 Other Homonuclear Double-Resonance Techniques 12.9 Complex Pulse Sequences 12.10 The 7-Modulated Spin Echo and the APT Experiment 12. 1 1 More About Polarization Transfer 12.12 Distortionless Enhancement by Polarization Transfer Chapter Summary References Additional Resources Review Problems
Chapter 13 TWO-DIMENSIONAL NUCLEAR MAGNETIC RESONANCE
13. 1 What is 2D NMR Spectroscopy? 13.2 2D Heteroscalar Shift-Correlated Spectra 13.3 2D Homonuclear Shift-Correlated Spectra 13.4 NOE Spectroscopy (NOESY) 13.5 Hetero- and Homonuclear 2D ./-Resolved Spectra 13.6 ID and 2D INADEQUATE 13.7 2D NMR Spectra of Systems Undergoing Exchange Chapter Summary References Additional Resources Review Problems
SELF-TEST II
Chapter 14 NMR STUDIES OF BIOLOGICALLY IMPORTANT MOLECULES
14. 1 Introduction 14.2 NMR Line Widths of Biopolymers 14.3 Exchangeable and Nonexchangeable Protons 14.4 Chemical Exchange 14.5 The Effects of pH on the NMR Spectra of Biomolecules 14.6 NMR Studies of Proteins 14.7 NMR Studies of Nucleic Acids 14.8 Lipids and Biological Membranes 14.9 Carbohydrates Chapter Summary References Additional Resources Review Problems
Chapter 15 SOLID-STATE NMR SPECTROSCOPY
15.1 Why Study Materials in the Solid State? 15.2 Why is NMR of Solids Different from NMR of Fluids? 15.3 Chemical Shifts in Solids 15.4 Spin-Spin Coupling 15.5 Quadrupole Coupling 297 15.6 Overcoming Long T\\ Cross Polarization Chapter Summary Additional Resources Review Problems
Chapter 16 NMR IN MEDICINE AND BIOLOGY: NMR IMAGING
16.1 A Window into Anatomy and Physiology 16.2 Biomedical NMR 16.3 Pictures with NMR: Magnetic Resonance Imaging 16.4 Image Contrast 16.5 Higher Dimensional Imaging 16.6 Chemical Shift Imaging 16.7 NMR Movies: Echo Planar Imaging 16.8 NMR Microscopy 16.9 In Vivo NMR Spectroscopy 16.10 Nonmedical Applications of MRI Chapter Summary Additional Resources
Appendix 1 ANSWERS TO REVIEW PROBLEMS
Appendix 2 PERIODIC TABLE
SUBJECT INDEX
CHEMICAL COMPOUNDS INDEX
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