Our attempt to present NMR spectroscopy to the beginner in a somewhat
different way was well-received, so that we were invited by Springer to make
some additions to the original for a second edition. Naturally we have modified
the text to take account of justified criticisms of the first edition. We decided
immediately to extend the number and scope of the problems section
comprising Part 2, as we know that this section has been very useful to our
readers. We felt that solid-state NMR is now so important and so relatively
easy to do that it would be well worth giving the reader a brief account of its
advantages and disadvantages. And, having already dealt with four important
nuclei in some detail, we decided to add some basic information on a number
of other spin-½ nuclei which are now often studied.
We thank Prof. Janet Blümel, Texas A&M University, and the Gesellschaft
Deutscher Chemiker for allowing us to reproduce solid state NMR spectra.
In addition we thank Klaus Jurkschat and Bernhard Lippert and their groups
for making available samples of organometallic molecules. Thanks also go to
Andrea Bokelmann and Bernhard Griewel for their valuable technical help.
Part 1: NMR Experiments 3
1 1D Experiments . 3
1.1 1H, D (2H): Natural Abundance, Sensitivity . 3
1.1.1 Proton NMR Spectrum of the Model Compound 1 . 4
1.1.2 Field Dependence of the Spectrum of 1 10
1.1.3 FID Manipulation: FT, EM, SINE BELL (CH2 Signal of 1) 11
1.1.4 The Proton Spectrum of 1 in D2O or H2O/D2O Mixtures . 14
1.1.5 Integration: Relaxation, T1, 90°-Pulse, Ernst Angle 16
1.1.6 The NOE: Through-Space Interactions between Protons 20
1.1.6.1 NOE Difference Spectroscopy 21
1.1.6.2 Selective 1D NOE Experiment (1D-NOESY) and Selective 1D
TOCSY Experiment . 22
1.2 13C 25
1.2.1 Natural Abundance 13C Spectrum of Compound 1 25
1.2.2 Coupled Spectrum (Gated Decoupling) . 28
1.2.3 Quantitative 13C Spectrum (Inverse Gated Decoupling) 29
1.2.4 Decoupled Spectrum: Proton Decoupling, Proton and Phosphorus
Decoupling 31
1.2.5 APT, DEPT, INEPT . 32
1.2.6 The INADEQUATE Experiment . 34
1.3 31P . 37
1.3.1 Natural Abundance 31P Spectrum of Compound 6 37
1.3.2 Proton-Decoupled and Proton-Coupled Spectra 37
1.3.3 Coupled Spectrum (P–P Coupling) 38
2 2D Experiments . 39
2.1 General Principles, Inverse Techniques, Gradients . 39
2.2 H,H COSY 41
2.3 2D NOE . 43
2.4 P,H COSY: with Varying Mixing Times for the Coupling 45
2.5 C,H Direct Correlation . 46
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