200 and More NMR Experiments: A Practical Course (2004)

Preface.Chapter 1: The NMR Spectrometer.1.1 Components of an NMR Spectrometer.1.1.1 The Magnet.1.1.2 The Spectrometer Cabinet.1.1.3 The Computer.1.1.4 Maintenance.1.2 Tuning a Probe-Head.1.3 The Lock Channel.1.4 The Art of Shimming.1.4.1 The Shim Gradients.1.4.2 The Shimming Procedure.1.4.3 Gradient Shimming.Chapter 2: Determination of Pulse-Duration.Exp. 2.1: Determination of the 90- 1H Transmitter Pulse-Duration.Exp. 2.2: Determination of the 90- 13C Transmitter Pulse-Duration.Exp. 2.3: Determination of the 90- 1H Decoupler Pulse-Duration.Exp. 2.4: The 90- 1H Pulse with Inverse Spectrometer Configuration.Exp. 2.5: The 90- 13C Decoupler Pulse with Inverse Configuration.Exp. 2.6: Composite Pulses.Exp. 2.7: Radiation Damping.Exp. 2.8: Pulse and Receiver Phases.Exp. 2.9: Determination of Radiofrequency Power.Chapter 3: Routine NMR Spectroscopy and Standard Tests.Exp. 3.1: The Standard 1H NMR Experiment.Exp. 3.2: The Standard 13C NMR Experiment.Exp. 3.3: The Application of Window Functions.Exp. 3.4: Computer-Aided Spectral Analysis.Exp. 3.5: Line Shape Test for 1H NMR Spectroscopy.Exp. 3.6: Resolution Test for 1H NMR Spectroscopy.Exp. 3.7: Sensitivity Test for 1H NMR Spectroscopy.Exp. 3.8: Line Shape Test for 13C NMR Spectroscopy.Exp. 3.9: ASTM Sensitivity Test for 13C NMR Spectroscopy.Exp. 3.10: Sensitivity Test for 13C NMR Spectroscopy.Exp. 3.11: Quadrature Image Test.Exp. 3.12: Dynamic Range Test for Signal Amplitudes.Exp. 3.13: 13- Phase Stability Test.Exp. 3.14: Radiofrequency Field Homogeneity.Chapter 4: Decoupling Techniques.Exp. 4.1: Decoupler Calibration for Homonuclear Decoupling.Exp. 4.2: Decoupler Calibration for Heteronuclear Decoupling.Exp. 4.3: Low-Power Calibration for Heteronuclear Decoupling.Exp. 4.4: Homonuclear Decoupling.Exp. 4.5: Homonuclear Decoupling at Two Frequencies.Exp. 4.6: The Homonuclear SPT Experiment.Exp. 4.7: The Heteronuclear SPT Experiment.Exp. 4.8: The Basic Homonuclear NOE Difference Experiment.Exp. 4.9: 1D Nuclear Overhauser Difference Spectroscopy.Exp. 4.10: 1D NOE Spectroscopy with Multiple Selective Irradiation.Exp. 4.11: 1H Off-Resonance Decoupled 13C NMR Spectra.Exp. 4.12: The Gated 1H-Decoupling Technique.Exp. 4.13: The Inverse Gated 1H-Decoupling Technique.Exp. 4.14: 1H Single-Frequency Decoupling of 13C NMR Spectra.Exp. 4.15: 1H Low-Power Decoupling of 13C NMR Spectra.Exp. 4.16: Measurement of the Heteronuclear Overhauser Effect.Chapter 5: Dynamic NMR Spectroscopy.Exp. 5.1: Low-Temperature Calibration Using Methanol.Exp. 5.2: High-Temperature Calibration Using 1,2-Ethanediol.Exp. 5.3: Dynamic 1H NMR Spectroscopy on Dimethylformamide.Exp. 5.4: The Saturation Transfer Experiment.Exp. 5.5: Measurement of the Rotating-Frame Relaxation Time T1rho.Chapter 6: 1D Multipulse Sequences.Exp. 6.1: Measurement of the Spin Lattice Relaxation Time T1.Exp. 6.2: Measurement of the Spin Spin Relaxation Time T2.Exp. 6.3: 13C NMR Spectra with SEFT.Exp. 6.4: 13C NMR Spectra with APT.Exp. 6.5: The Basic INEPT Technique.Exp. 6.6: INEPT+.Exp. 6.7: Refocused INEPT.Exp. 6.8: Reverse INEPT.Exp. 6.9: DEPT-135.Exp. 6.10: Editing 13C NMR Spectra Using DEPT.Exp. 6.11: DEPTQ.Exp. 6.12: Multiplicity Determination Using PENDANT.Exp. 6.13: 1D-INADEQUATE.Exp. 6.14: The BIRD Filter.Exp. 6.15: TANGO.Exp. 6.16: The Heteronuclear Double-Quantum Filter.Exp. 6.17: Purging with a Spin-Lock Pulse.Exp. 6.18: Water Suppression by Presaturation.Exp. 6.19: Water Suppression by the Jump-and-Return Method.Chapter 7: NMR Spectroscopy with Selective Pulses.Exp. 7.1: Determination of a Shaped 90- 1H Transmitter Pulse.Exp. 7.2: Determination of a Shaped 90- 1H Decoupler Pulse.Exp. 7.3: Determination of a Shaped 90- 13C Decoupler Pulse.Exp. 7.4: Selective Excitation Using DANTE.Exp. 7.5: SELCOSY.Exp. 7.6: SELINCOR: Selective Inverse H,C Correlation via 1J(C,H).Exp. 7.7: SELINQUATE.Exp. 7.8: Selective TOCSY.Exp. 7.9: INAPT.Exp. 7.10: Determination of Long-Range C,H Coupling Constants.Exp. 7.11: SELRESOLV.Exp. 7.12: SERF.Chapter 8: Auxiliary Reagents, Quantitative Determinations, and Reaction Mechanisms.Exp. 8.1: Signal Separation Using a Lanthanide Shift Reagent.Exp. 8.2: Signal Separation of Enantiomers Using a Chiral Shift Reagent.Exp. 8.3: Signal Separation of Enantiomers Using a Chiral Solvating Agent.Exp. 8.4: Determination of Enantiomeric Purity with Pirkle's Reagent.Exp. 8.5: Determination of Enantiomeric Purity by 31P NMR.Exp. 8.6: Determination of Absolute Configuration by the AdvancedMosher Method.Exp. 8.7: Aromatic Solvent-Induced Shift (ASIS).Exp. 8.8: NMR Spectroscopy of OH Protons and H/D Exchange.Exp. 8.9: Water Suppression Using an Exchange Reagent.Exp. 8.10: Isotope Effects on Chemical Shielding.Exp. 8.11: pKa Determination by 13C NMR.Exp. 8.12: Determination of Association Constants Ka.Exp. 8.13: Saturation Transfer Difference NMR.Exp. 8.14: The Relaxation Reagent Cr(acac)3.Exp. 8.15: Determination of Paramagnetic Susceptibility by NMR.Exp. 8.16: 1H and 13C NMR of Paramagnetic Compounds.Exp. 8.17: The CIDNP Effect.Exp. 8.18: Quantitative 1H NMR Spectroscopy: Determination of the Alcohol Content of Polish Vodka.Exp. 8.19: Quantitative 13C NMR Spectroscopy with Inverse Gated 1H-Decoupling.Exp. 8.20: NMR Using Liquid-Crystal Solvents.Chapter 9: Heteronuclear NMR Spectroscopy.Exp. 9.1: 1H-Decoupled 15N NMR Spectra Using DEPT.Exp. 9.2: 1H-Coupled 15N NMR Spectra Using DEPT.Exp. 9.3: 19F NMR Spectroscopy.Exp. 9.4: 29Si NMR Spectroscopy Using DEPT.Exp. 9.5: 29Si NMR Spectroscopy Using Spin-Lock Polarization.Exp. 9.6: 119Sn NMR Spectroscopy.Exp. 9.7: 2H NMR Spectroscopy.Exp. 9.8: 11B NMR Spectroscopy.Exp. 9.9: 17O NMR Spectroscopy Using RIDE.Exp. 9.10: 47/49Ti NMR Spectroscopy Using ARING.Chapter 10: The Second Dimension.Exp. 10.1: 2D J-Resolved 1H NMR Spectroscopy.Exp. 10.2: 2D J-Resolved 13C NMR Spectroscopy.Exp. 10.3: The Basic H,H-COSY Experiment.Exp. 10.4: Long-Range COSY.Exp. 10.5: Phase-Sensitive COSY.Exp. 10.6: Phase-Sensitive COSY-45.Exp. 10.7: E.COSY.Exp. 10.8: Double-Quantum-Filtered COSY with Presaturation.Exp. 10.9: Fully Coupled C,H Correlation (FUCOUP).Exp. 10.10: C,H-Correlation by Polarization Transfer (HETCOR).Exp. 10.11: Long-Range C,H-Correlation by Polarization Transfer.Exp. 10.12: C,H Correlation via Long-Range Couplings (COLOC).Exp. 10.13: The Basic HMQC Experiment.Exp. 10.14: Phase-Sensitive HMQC with BIRD Filter and GARP Decoupling.Exp. 10.15: Poor Man's Gradient HMQC.Exp. 10.16: Phase-Sensitive HMBC with BIRD Filter.Exp. 10.17: The Basic HSQC Experiment.Exp. 10.18: The HOHAHA or TOCSY Experiment.Exp. 10.19: HETLOC.Exp. 10.20: The NOESY Experiment.Exp. 10.21: The CAMELSPIN or ROESY Experiment.Exp. 10.22: The HOESY Experiment.Exp. 10.23: 2D-INADEQUATE.Exp. 10.24: The EXSY Experiment.Exp. 10.25: X,Y-Correlation.Chapter 11: 1D NMR Spectroscopy with Pulsed Field Gradients.Exp. 11.1: Calibration of Pulsed Field Gradients.Exp. 11.2: Gradient Pre-emphasis.Exp. 11.3: Gradient Amplifier Test.Exp. 11.4: Determination of Pulsed Field Gradient Ring-Down Delays.Exp. 11.5: The Pulsed Field Gradient Spin-Echo Experiment.Exp. 11.6: Excitation Pattern of Selective Pulses.Exp. 11.7: The Gradient Heteronuclear Double-Quantum Filter.Exp. 11.8: The Gradient zz-Filter.Exp. 11.9: The Gradient-Selected Dual Step Low-Pass Filter.Exp. 11.10: gs-SELCOSY.Exp. 11.11: gs-SELTOCSY.Exp. 11.12: DPFGSE-NOE.Exp. 11.13: gs-SELINCOR.Exp. 11.14: alpha/beta-SELINCOR-TOCSY.Exp. 11.15: GRECCO.Exp. 11.16: WATERGATE.Exp. 11.17: Water Suppression by Excitation Sculpting.Exp. 11.18: Solvent Suppression Using WET.Exp. 11.19: DOSY.Exp. 11.20: INEPT-DOSY.Exp. 11.21: DOSY-HMQC.Chapter 12: 2D NMR Spectroscopy With Field Gradients.Exp. 12.1: gs-COSY.Exp. 12.2: Constant-Time COSY.Exp. 12.3: Phase-Sensitive gs-DQF-COSY.Exp. 12.4: gs-HMQC.Exp. 12.5: gs-HMBC.Exp. 12.6: ACCORD-HMBC.Exp. 12.7: HMSC.Exp. 12.8: Phase-Sensititive gs-HSQC with Sensitivity Enhancement.Exp. 12.9: Edited HSQC with Sensitivity Enhancement.Exp. 12.10: HSQC with Adiabatic Pulses for High-Field Instruments.Exp. 12.11: gs-TOCSY.Exp. 12.12: gs-HMQC-TOCSY.Exp. 12.13: gs-HETLOC.Exp. 12.14: gs-J-Resolved HMBC.Exp. 12.15: 2Q-HMBC.Exp. 12.16: 1H-Detected 2D INEPT-INADEQUATE.Exp. 12.17: 1,1-ADEQUATE.Exp. 12.18: 1,n-ADEQUATE.Exp. 12.19: gs-NOESY.Exp. 12.20: gs-HSQC-NOESY.Exp. 12.21: gs-HOESY.Exp. 12.22: 1H,15N Correlation with gs-HMQC.Chapter 13: The Third Dimension.Exp. 13.1: 3D HMQC-COSY.Exp. 13.2: 3D gs-HSQC-TOCSY.Exp. 13.3: 3D H,C,P-Correlation.Exp. 13.4: 3D HMBC.Chapter 14: Solid-State NMR Spectroscopy.Exp. 14.1: Shimming Solid-State Probe-Heads.Exp. 14.2: Adjusting the Magic Angle.Exp. 14.3: Hartmann Hahn Matching.Exp. 14.4: The Basic CP/MAS Experiment.Exp. 14.5: TOSS.Exp. 14.6: SELTICS.Exp. 14.7: Connectivity Determination in the Solid State.Exp. 14.8: REDOR.Exp. 14.9: High-Resolution Magic-Angle Spinning.Chapter 15: Protein NMR.Exp. 15.1: Pulse Determination for Protein NMR.Exp. 15.2: HN-HSQC.Exp. 15.3: HC-HSQC.Exp. 15.4: MUSIC.Exp. 15.5: HN-Correlation using TROSY.Exp. 15.6: HN-TOCSY-HSQC.Exp. 15.7: HNCA.Exp. 15.8: HN(CO)CA.Exp. 15.9: HNCO.Exp. 15.10: HN(CA)CO.Exp. 15.11: HCACO.Exp. 15.12: HCCH-TOCSY.Exp. 15.13: CBCANH.Exp. 15.14: CBCA(CO)NH.Exp. 15.15: HBHA(CBCACO)NH.Exp. 15.16: HN(CA)NNH.Exp. 15.17: HN-NOESY-HSQC.Exp. 15.18: HC-NOESY-HSQC.Exp. 15.19: 3D HCN-NOESY.Exp. 15.20: HNCA-J.Appendix 1: Pulse Programs.Appendix 2: Instrument Dialects.Appendix 3: Classification of Experiments.Appendix 4: Elementary Product Operator Formalism Rules.Appendix 5: Chemical Shift and Spin-Coupling Data for Ethyl Crotonate and Strychnine.Glossary and Index.