Applied NMR Spectroscopy for Chemists and Life Scientists

Technical Aspects of NMRTHE COMPONENTS OF AN NMR SPECTROMETERThe MagnetShim Systems and ShimmingThe ElectronicsThe ProbeheadThe Lock SystemProblemsACQUISITION AND PROCESSINGThe Time Domain SignalFourier TransformTechnical Details of Data AcquisitionData ProcessingProblemsEXPERIMENTAL TECHNIQUESRF PulsesPulsed Field GradientsPhase CyclingDecouplingIsotropic MixingSolvent SuppressionBasic 1D ExperimentsMeasuring Relaxation TimesThe INEPT ExperimentThe DEPT ExperimentProblemsTHE ART OF PULSE EXPERIMENTSIntroductionOur Toolbox: Pulses, Delays, and Pulsed Field GradientsThe Excitation BlockThe Mixing PeriodSimple Homonuclear 2D SequencesHeteronuclear 2D Correlation ExperimentsExperiments for Measuring Relaxation TimesTriple-Resonance NMR ExperimentsExperimental DetailsProblemsPART FOUR - Important Phenomena and Methods in Modern NMRRELAXATIONIntroductionRelaxation: The Macroscopic PictureThe Microscopic Picture: Relaxation MechanismsRelaxation and MotionMeasuring 15N Relaxation to Determine Protein DynamicsMeasurement of Relaxation DispersionProblemsTHE NUCLEAR OVERHAUSER EFFECTIntroductionThe Formal Description of the NOE: The Solomon EquationsApplications of the NOE in Stereochemical AnalysisPractical Tips for Measuring NOEsProblemsCHEMICAL AND CONFORMATIONAL EXCHANGETwo-Site ExchangeExperimental Determination of the Rate ConstantsDetermination of the Activation Energy by Variable-Temperature NMR ExperimentsProblemsTWO-DIMENSIONAL NMR SPECTROSCOPYIntroductionThe Appearance of 2D SpectraTwo-Dimensional NMR Spectroscopy: How Does It Work?Types of 2D NMR ExperimentsThree-Dimensional NMR SpectroscopyPractical Aspects of Measuring 2D SpectraProblemsSOLID-STATE NMR EXPERIMENTSIntroductionThe Chemical Shift in the Solid StateDipolar Couplings in the Solid StateRemoving CSA and Dipolar Couplings: Magic-Angle SpinningReintroducing Dipolar Couplings under MAS ConditionsPolarization Transfer in the Solid State: Cross-PolarizationTechnical Aspects of Solid-State NMR ExperimentsProblemsDETECTION OF INTERMOLECULAR INTERACTIONSIntroductionChemical Shift PerturbationMethods 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 MethodsProblemsPART FIVE - Structure Determination of Natural Products by NMRCARBOHYDRATESThe Chemical Nature of CarbohydratesNMR Spectroscopy of CarbohydratesQuick IdentificationA Worked Example: SucroseSTEROIDSIntroductionA Worked Example: PrednisonePEPTIDES AND PROTEINSIntroductionThe Structure of Peptides and ProteinsNMR of Peptides and ProteinsAssignment of Peptide and Protein ResonancesA Worked Example: The Pentapeptide TP5NUCLEIC ACIDSIntroductionThe Structure of DNA and RNANMR of DNA and RNAAssignment of DNA and RNA ResonancesAPPENDIXThe Magnetic H and B FieldsMagnetic Dipole Moment and MagnetizationScalars, Vectors, and TensorsProperties of Matrices