50 and More Essential NMR Experiments

[Book Description]

 This book is the perfect link for learning how to perform the experiments after only having studied theory. In eight chapters more than 50 essential NMR experiments are described in detail. Special focus is put on the organic set of NMR spectra (1H, 13C-APT, COSY, NOESY, HSQC and HMBC). Different chapters deal with advanced organic NMR, selective methods, heteronuclear NMR, relaxation and diffusion measurements, organic applications and maintenance. Every experiment has a section providing the reader with the purpose and scope of the specific experiment. Every experiment is concluded with the spectrum as it is obtained under the conditions described. Questions and comments enable the reader to check their understanding. The authors are very experienced and the whole book is in full color, which enhances the reading experience and makes the spectra and other figures easier to understand. This book is strongly recommended for all students and researchers who are involved in the structural elucidation of chemical compounds both in practical education and in pursuing research, in particular if they handle an NMR spectrometer.

[Table of Contents]

Preface
    Chapter 1 The Organic Set of NMR Spectra       1  (34)
      1.1 The 1H NMR Experiment                    3  (4)
      1.2 APT-13C NMR                              7  (4)
      1.3 Cosy                                     11 (6)
      1.4 Noesy                                    17 (6)
      1.5 Hsqc                                     23 (6)
      1.6 Hmbc                                     29 (6)
    Chapter 2 Advanced Organic NMR Spectroscopy    35 (40)
      2.1 2D J-Resolved 1H NMR Spectroscopy        37 (4)
      2.2 Roesy                                    41 (4)
      2.3 Tocsy                                    45 (4)
      2.4 Hsqc-Tocsy                               49 (4)
      2.5 Hoesy                                    53 (4)
      2.6 Inadequate                               57 (4)
      2.7 Adequate                                 61 (4)
      2.8 J-HMBC                                   65 (6)
      2.9 Gated Decoupling                         71 (4)
    Chapter 3 Selective Methods                    75 (38)
      3.1 Water suppression by Presaturation       77 (4)
      3.2 Solvent Suppression by 1D-NOESY          81 (4)
      3.3 Water Suppression by SOGGY Excitation    85 (4)
      Sculpting
      3.4 Solvent Suppression using WET            89 (4)
      3.5 Seltocsy                                 93 (4)
      3.6 Selnoesy                                 97 (4)
      3.7 Selincor                                 101(4)
      3.8 Selinquate                               105(4)
      3.9 Band Selective HMBC                      109(4)
    Chapter 4 Heteronuclear NMR                    113(36)
      4.1 11B NMR Spectroscopy                     119(4)
      4.2 15N NMR Spectroscopy                     123(4)
      4.3 17O NMR Spectroscopy                     127(4)
      4.4 19F NMR Spectroscopy                     131(4)
      4.5 29Si NMR Spectroscopy                    135(4)
      4.6 57Fe NMR Spectroscopy                    139(6)
      4.7 195Pt NMR Spectroscopy                   145(4)
    Chapter 5 Experiments in Physical Organic      149(24)
    Chemistry
      5.1 Measurement of the Spin--Lattice         151(4)
      Relaxation Time T1
      5.2 Measurement of the Spin--Spin            155(4)
      Relaxation Time T2
      5.3 Dynamic 1H NMR Spectroscopy              159(4)
      5.4 Diffusion Measurement with DOSY          163(4)
      5.5 Residual Dipolar Couplings (RDC)         167(6)
    Chapter 6 Organic Chemistry Applications       173(36)
      6.1 ASIS                                     175(4)
      6.2 Chirality Determination                  179(4)
      6.3 Advanced Mosher Method                   183(4)
      6.4 Quantitative NMR and Relaxation          187(6)
      Reagents
      6.5 Determination of Association             193(6)
      Constants Ka
      6.6 STD NMR                                  199(4)
      6.7 A Kinetic Experiment                     203(6)
    Chapter 7 An Excursion to the Solid State      209(24)
    and to Structural Biology
      7.1 The CP/MAS Experiment                    211(4)
      7.2 High-Resolution Magic-Angle Spinning     215(4)
      7.3 HN-HSQC                                  219(6)
      7.4 HNCA                                     225(8)
    Chapter 8 Maintenance and Calibration          233(40)
      8.1 Calibration of Pulse Duration in the     235(6)
      Transmitter Channel
      8.2 Calibration of the Pulse Duration in     241(6)
      the Indirect Channel
      8.3 Shaped Pulses                            247(6)
      8.4 Adiabatic pulses                         253(4)
      8.5 Temperature Calibration in NMR           257(8)
      8.6 Calibration of Pulsed Field Gradients    265(8)
  Appendix
Answers                                            273(22)
Pulse Programs                                     295(1)
Elementary Product Operator Formalism Rules        296(2)
Chemical Shift and Spin-Coupling Data for          298(2)
Strychnine
Picture Credits                                    300(1)
Index                                              301