Applied NMR Spectroscopy for Chemists and Life Scientists

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