NMR--from spectra to structures : an experimental approach / Terence N. Mitchell, Burkhard Costisella.

Format:

Book

Author/Creator:

Mitchell, Terence N.

Contributor:

Costisella, Burkhard.

Hazel M. Hussong Fund.

Language:

English

Subjects (All):

Nuclear magnetic resonance spectroscopy.

Physical Description:

xiii, 207 pages : illustrations ; 24 cm

Edition:

Second revised and expanded edition.

Place of Publication:

Berlin ; New York : Springer, [2007]

Summary:

Nuclear magnetic resonance spectroscopy is one of the most powerful analytical methods. This practice-oriented textbook aims at teaching how NMR experiments should be used to make structural asssignments. The book is intended as a practical guide for students and laboratory personnel, so that the emphasis is on practical rather than on theoretical aspects, which are treated only to the extent necessary to understand the basis of the experiments. and to interpret the results.

The second edition has been expanded to include several other heteronuclei ([superscript 15]N, [superscript 19]F, [superscript 29]Si, [superscript 77]Se, [superscript 113]Cd, [superscript 117]Sn/[superscript 119]Sn, [superscript 195]Pt, [superscript 207]Pb) and a new chapter on solid state NMR. The problems section has been enlarged and now includes 50 problems. These are of different degrees of complexity and in all cases include two-dimensional (2D) methods as well as standard proton and carbon 1D spectra.

Contents:

Part 1 NMR Experiments 3

1 1D Experiments 3

1.1 [superscript 1]H, D ([superscript 2]H): 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 (CH[subscript 2] Signal of 1) 11

1.1.4 The Proton Spectrum of 1 in D[subscript 2]O or H[subscript 2]O/D[subscript 2]O Mixtures 14

1.1.5 Integration: Relaxation, T[subscript 1] 90[superscript degree]-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 [superscript 13]C 25

1.2.1 Natural Abundance [superscript 13]C Spectrum of Compound 1 25

1.2.2 Coupled Spectrum (Gated Decoupling) 28

1.2.3 Quantitative [superscript 13]C 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 [superscript 31]P 37

1.3.1 Natural Abundance [superscript 31]P 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

2.6 C,H Long Range Correlation 47

2.7 P,C Correlation 48

2.8 P,P Correlation 50

3 Quadrupolar Nucleus Experiments 51

3.1 General Principles: Quadrupole Moment, Relaxation, Linewidth 51

3.2 [superscript 17]O 51

3.2.1 [superscript 17]O Spectrum of 7: Chemical Shift (Reference), Coupling with P 52

3.2.2 P-O Correlation 52

4 HPLC-NMR Coupling 53

4.1 General Principles, NMR as a Highly Sensitive Analytical Tool ([Mu]g to ng Amounts) 53

4.2 Example: Separation of 4 and 5, Two Acetals of Formylphosphonic Ester 54

4.3 Chromatogram 54

4.4 On-Flow Diagram (Chemical Shift vs. Time) 55

4.5 Stopped Flow Experiments 58

5 Other Spin-[fraction 12] Nuclei 59

5.1 [superscript 15]N 60

5.2 [superscript 19]F 62

5.3 [superscript 29]Si 62

5.4 [superscript 77]Se 66

5.5 [superscript 113]Cd 67

5.6 [superscript 117]Sn, [superscript 119]Sn 67

5.7 [superscript 195]Pt 69

5.8 [superscript 207]Pb 72

6 Solid State NMR 73

6.2 Solid State [superscript 1]H NMR 74

6.3 Solid State [superscript 13]C NMR 75

6.4 Solid-State [superscript 31]P NMR 77

6.5 Solid-State [superscript 29]Si NMR 81

6.6 Solid State NMR 81

Appendix Reference List 84

Part 2 Worked Example and Problems 85

Solving the Structures of Organic Molecules 85

Elemental Analysis 86

Mass Spectrometry 86

2.2 Worked Example 88

H,H Correlation 89

C,H Correlation 89

2.3 Problems 93

Problems 166.

Notes:

Includes bibliographical references (page 84).

Local Notes:

Acquired for the Penn Libraries with assistance from the Hazel M. Hussong Fund.

ISBN:

3540721959

9783540721956

OCLC:

153582148