Chapter 7 – NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY

Most chapters end with an Additional Reading section. 1. Basic Theory of NMR Spectroscopy. Nuclear Spin. Interaction of Nuclear spins with Magnetic Fields. Precession and Larmour Frequency. Nuclear Energy Levels and Relaxation. The Rotating Frame of Reference. The Bloch Equations. 2. Measurement of the Spectrum-Instrumentation. Fundamental Components of an NMR Spectrometer. The Magnet. The Transmitter Coil. The Receiver Coil. The Sample. Obtaining a Spectrum. Continuous-Wave Experiments. Fourier Transform Experiments. Detecting the Signal and Digitizing the Data. Processing the Signal. The Fourier Transformation Process. Double and Triple Resonance. Homonuclear Decoupling. Heteronuclear Decoupling. Pulse Sequences. Signal-to-Noise Ratio. 3. The Chemical Shift and Examples for Selected Nuclei. General Considerations. Protein Chemical Shifts. Carbon Chemical Shifts. Boron Chemical Shifts. Nitrogen Chemical Shifts. Flourine Chemical Shifts. Phosphorous Chemical Shifts. Platinum Chemical Shifts. 4. Symmetry and NMR Spectroscopy. Introduction. Spin-System Designation. 5. Spin-Spin Coupling and NMR Spin Systems. General considerations. Quantum Mechanics and NMR Spectroscopy. 6. Typical Magnitude of Selected Coupling Constants. General Considerations. Vicinal (3JHH) Couplings. Geminal (2JHH) Couplings. Long Range H-H Couplings. 1JCH Couplings. 2JCH and 3JCH Couplings. nJCC Couplings. nJNH and 3JNC Couplings. nJFX Couplings. nJPX Couplings. 7. Nuclear Spin Relaxation. Introduction. Different Types of Relaxation. Microscopic Origin of Relaxation. Different Types of Relaxation Mechanisms. Experimental Behavior of Nuclear Relaxation. Experimental Measurement of Relaxation Times. The 13C Nucleus and Its Dominant Relaxation Mechanisms. 8. The Nuclear Overhauser Effect. Introduction. Experimental Measurement. 9. Editing 13C NMR Spectra. Introduction. Attached-Proton Test (APT). Distortionless Enhancement by Polarization Transfer (DEPT). 10. Two-Dimensional NMR Spectroscopy. Introduction. The Basic Two-Dimensional NMR Experiment. Graphical Presentation of 2D NMR Spectra. Two-Dimensional I-Resolved Spectroscopy. Two-Dimensional Correlated Spectroscopy. Two-Dimensional Exchange Spectroscopy (NOESY and EXSY). The Two-dimensional INADEQUATE Experiment. HMQC and HMBC Spectra. Data Acquisition and Processing Parameters in 2D NMR Spectroscopy. 11. Dynamic NMR Spectroscopy. Introduction. Determination of Exchange Rates. Coalescence Temperatures and Rate Constants at Coalescence. Complete Line-Shape Analysis. Activation Parameters. Equilibrium Thermodynamics. Examples of Dynamic Processes Studied by NMR Spectroscopy. 12. Lanthanide Shift Reagents (LSR). Introduction. Theory of Shift Reagent-Substrate Interaction. Contact and Depolar Interactions. Dtermination of Molecular Geometry. Chiral Lanthanide-Shift Reagents. Practical Considerations. 13. NMR of Solids. Introduction. Proton Dipolar Broadening. Chemical-Shift Anisotropy. Magic-Angles Spinning. Cross Polarization. Recapitualization. Crystallographic Equivalence, Chemical-Shift Equivalence, and Magnetic Equivalence in CP/MAS NMR Spectra. Molecular Motion in the Solid State. 14. Problems. Problems. Appendix A: Selected Values of Longitudinal Relaxation Times for Some Nuclei. Index.