Table of Contents
Preface
Chapter 1 The Organic Set of NMR Spectra 1
1.1 The 1H NMR Experiment 3
1.2 Apt-13C NMR 7
1.3 COSY 11
1.4 NOESY 17
1.5 HSQC 23
1.6 HMBC 29
Chapter 2 Advanced Organic NMR Spectroscopy 35
2.1 2D J-Resolved 1H NMR Spectroscopy 37
2.2 ROESY 41
2.3 TOCSY 45
2.4 HSQC-TOCSY 49
2.5 HOESY 53
2.6 INADEQUATE 57
2.7 ADEQUATE 61
2.8 J-HMBC 65
2.9 Gated Decoupling 71
Chapter 3 Selective Methods 75
3.1 Water suppression by Presaturation 77
3.2 Solvent Suppression by 1D-NOESY 81
3.3 Water Suppression by SOGGY Excitation Sculpting 85
3.4 Solvent Suppression using WET 89
3.5 SELTOCSY 93
3.6 SELNOESY 97
3.7 SELINCOR 101
3.8 SELINQUATE 105
3.9 Band Selective HMBC 109
Chapter 4 Heteronuclear NMR 113
4.1 11B NMR Spectroscopy 119
4.2 15N NMR Spectroscopy 123
4.3 17O NMR Spectroscopy 127
4.4 19F NMR Spectroscopy 131
4.5 29Si NMR Spectroscopy 135
4.6 57Fe NMR Spectroscopy 139
4.7 195Pt NMR Spectroscopy 145
Chapter 5 Experiments in Physical Organic Chemistry 149
5.1 Measurement of the Spin–Lattice Relaxation Time T1 151
5.2 Measurement of the Spin–Spin Relaxation Time T2 155
5.3 Dynamic 1H NMR Spectroscopy 159
5.4 Diffusion Measurement with DOSY 163
5.5 Residual Dipolar Couplings (RDC) 167
Chapter 6 Organic Chemistry Applications 173
6.1 ASIS 175
6.2 Chirality Determination 179
6.3 Advanced Mosher Method 183
6.4 Quantitative NMR and Relaxation Reagents 187
6.5 Determination of Association Constants Ka 193
6.6 STD NMR 199
6.7 A Kinetic Experiment 203
Chapter 7 An Excursion to the Solid State and to Structural Biology 209
7.1 The CP/MAS Experiment 211
7.2 High-Resolution Magic-Angle Spinning 215
7.3 HN-HSQC 219
7.4 HNCA 225
Chapter 8 Maintenance and Calibration 233
8.1 Calibration of Pulse Duration in the Transmitter Channel 235
8.2 Calibration of the Pulse Duration in the Indirect Channel 241
8.3 Shaped Pulses 247
8.4 Adiabatic pulses 253
8.5 Temperature Calibration in NMR 257
8.6 Calibration of Pulsed Field Gradients 265
Appendix
Answers 273
Pulse Programs 295
Elementary Product Operator Formalism Rules 296
Chemical Shift and Spin-Coupling Data for Strychnine 298
Picture Credits 300
Index 301
