Basic One- and Two-Dimensional NMR Spectroscopy
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1 F Horst Friebolin eplained s emistry Basic One- and Two-Dimensional NMR Spectroscopy Sth completely revised and enlarged edition ~ WILEY~ VCH WILEY-VCH Verlag GmbH & Co. KGaA
2 p Contents The Physical Basis of NMR Spectroscopy Introduction Nuclear Angular Momentum and Magnetic Moment Nuclei in a Static Magnetic Field Directional Quantization Energy of the Nuclei in the Magnetic Field.... Populations of the Energy Levels.... Macroscopic Magnetization Basic Principles of the NMR Experiment.... The Resonance Condition Basic Principle of the NMR Measurement.... The Pulsed NMR Method The Pulse The Pulse Angle Relaxation The Time and Frequency Domains; the Fourier Transformation Spectrum Accumulation The Pulsed NMR Spectrometer.... Spectral Parameters: a Brief Survey..... The Chemical Shift Nuclear Shielding Reference Compounds and the a-scale Spin-Spin Coupling The Indirect Spin-Spin Coupling Coupling to One Neighboring Nucleus (AX Spin System) Coupling to Two Equivalent Neighboring Nuclei (AX2 Spin System) Coupling to Three or More Equivalent Neighboring Nuclei (AXn Spin System)..... Multiplicity Rules Couplings between Three Non-equivalent Nuclei (AMX Spin System) Couplings between Equivalent Nuclei (An Spin Systems) The Order of a Spectrum Basic One- and Two-Dimensional Spectroscopy. 5th Edition. Horst Friebolin Copyright 2011 WILEY-VCR Verlag GmbH & Co. KGaA, Weinheim ISBN XVII
3 Couplings between Protons and other Nuclei ; 13 C Satellite Spectra... The Intensities of the Resonance Signals H Signal Intensities C Signal Intensities Summary "Other" Nuclides Nuclides with Spin I = 1/2.... Nuclides with Spin I > Exercises Bibliography for Chapter The Chemical Shift Introduction.... Influence of the Charge Density on the Shielding Effects of Neighboring Groups Magnetic Anisotropy of Neighboring Groups.. Ring Current Effects.... Electric Field Effects Intermolecular Interactions - Hydrogen Bonding and Solvent Effects.... Isotope Effects Summary H Chemical Shifts of Organic Compounds... Alkanes and Cycloalkanes Alkenes Arenes Alkynes.... Aldehydes OH,SH,NH C Chemical Shifts of Organic Compounds... Alkanes and Cycloalkanes Alkenes.... Arenes Alkynes.... Allenes.... Carbonyl and Carboxy Compounds.... Aldehydes and Ketones Carboxylic Acids and Derivatives.... Relationships between the Spectrum and the Molecular Structure Equivalence, Symmetry and Chirality.... Homotopic, Enantiotopic and Diastereotopic Groups Summary Chemical Shifts of "Other" Nuclides.... Exercises Bibliography for Chapter Indirect Sp Introduction H,H Couplir Structure.. Geminal Cm Dependence Substituent I Effects of Nc Vicinal Coup Dependence Substituent I H,H Couplir Long-range ( C,H Couplin Chemical Str C,H Couplin Dependence Substituent E C,H Couplin Geminal Cm (i.e. 2 J(C,H: Vicinal Coup (i.e. 3 J(C,Hl Long-range < C,H Couplin C,C Couplin; Chemical Str Correlations Constants.. Coupling Me The Electron H,D Couplin Relationship Lifetime of a Couplings tlu Couplings o~ (Heteronucle Exercises.. Bibliography Spectrum A Introduction Nomenclatur Systematic N Chemical anc Tho-Spin Sy! The AX Spin The AB Spin XVIII
4 Indirect Spin-Spin Coupling.... Introduction JI,H Coupling Constants and Chemical Structure Geminal Couplings 2 J(H,H) Dependence on Bond Angle..... Substituent Effects..... Effects of Neighboring n-electrons Vicinal Couplings 3 1 (H,H)..... Dependence on the Dihedral Angle.... Substituent Effects H,H Couplings in Aromatic Compounds.... Long-range Couplings C,H Coupling Constants and Chemical Structure C,H Couplings through One Bond 1 J(C,H)... Dependence on the s-fraction Substituent Effects C,H Couplings through 1\vo or More Bonds... Geminal Couplings (i.e. 2 J(C,H) in H-C- 13 C) Vicinal Couplings (i.e. 3 J(C,H) in H-C-C- BC) Long-range Couplings 3 +nj(c,h)..... C,H Couplings in Benzene Derivatives.... C,C Coupling Constants and Chemical Structure Correlations between C,H and H,H Coupling Constants Coupling Mechanisms The Electron-Nuclear Interaction H,D Couplings Relationship between the Coupling and the Lifetime of a Spin State Couplings through Space Couplings of "Other" Nuclides (Heteronuclear Couplings) Exercises Bibliography for Chapter Spectrum Analysis and Calculations... Introduction Nomenclature Systematic Notation for Spin Systems.... Chemical and Magnetic Equivalence Two-Spin Systems The AX Spin System The AB Spin System XIX
5 Three-Spin Systems y 1 Measurement The AX 2, AKz, ABz and A3 Spin Systems Chemical Change The AMX and ABX Spin Systems Solvent and Tern Four-Spin Systems Shift Reagents AzX 2 and AzBz Spin Systems Computer-aided The AA'XX' and AA'BB' Spin Systems of nc NMR Spe 4.6 Spectrum Simulation and Iteration Searching for Ide 4.7 Analysis of 13 C NMR Spectra Spectrum Predic Exercises Exercises Bibliography for Chapter Bibliography for 5 Double Resonance Experiments Relaxation Introduction Introduction Spin Decoupling in 1 H NMR Spectroscopy Spin-Lattice Rei Simplification of Spectra Relaxation Mecl by Selective Spin Decoupling Experimental D Suppression of a Solvent Signal the Inversion Rc 5.3 Spin Decoupling in 13 C NMR Spectroscopy Relationships b< H Broad-band Decoupling and Chemical S The Gated Decoupling Experiment Influence of Pre H Off-Resonance Decoupling Groups Selective Decoupling Influence of Me in 13 C NMR Spectroscopy Segmental Mob Exercises Anisotropy of tl 5.4 Bibliography for Chapter Suppression of 7.3 Spin-Spin Relru 6 Assignment of 1 H and 13 C Signals Relaxation Me< 6.1 Introduction Experimental I 6.2 lh NMR Spectroscopy the Spin-Echo Defining the Problem Line-widths of: Empirical Correlations for Exercises... Predicting Chemical Shifts Bibliography f Alkanes (Shoolery's Rule) Alkenes One-Dimensi Benzene Derivatives using Complc Decoupling Experiments Introduction Altering the Chemical Structure of the Sample Basic Techniq Effects of Solvent and Temperature Pulsed Field G Shift Reagents The Effect of t Lanthanide Shift Reagents (LSRs) Magnetization Chiral Lanthanide Shift Reagents The Effect of t 6.3 DC NMR Spectroscopy on the Transvf Defining the Problem (Mx, My ) Empirical Correlations for Predicting Spin-Locking Approximate Chemical Shifts The Effect of l Alkanes Transverse M~ Alkenes The J-Modula Benzene Derivatives The Pulsed G Decoupling Experiments Signal Enhan< XX
6 y 1 Measurements Chemical Changes to the Sample Solvent and Temperature Effects and Shift Reagents Computer-aided Assignment of 13C NMR Spectra Searching for Identical or Related Compounds 161 Spectrum Prediction Exercises Bibliography for Chapter Relaxation Introduction Spin-Lattice Relaxation of13 C Nuclei (T1) Relaxation Mechanisms Experimental Determination of T1; the Inversion Recovery Experiment Relationships between T1 and Chemical Structure Influence of Protons inch, CH2 and CH Groups Influence of Molecular Size..... Segmental Mobilities Anisotropy of the Molecular Mobility Suppression of the Water Signal Spin-Spin Relaxation (T 2 ) Relaxation Mechanisms Experimental Determination of T 2 ; the Spin-Echo Experiment Line-widths of NMR Signals Exercises Bibliography for Chapter One-Dimensional NMR Experiments using Complex Pulse Sequences Introduction Basic Techniques Using Pulse Sequences and Pulsed Field Gradients The Effect of the Pulse on the Longitudinal Magnetization (Mz) The Effect of the Pulse on the Transverse Magnetization Components (Mx, My ) Spin-Locking The Effect of Pulsed Field Gradients on the Transverse Magnetization The ]-Modulated Spin-Echo Experiment The Pulsed Gradient Spin-Echo Experiment Signal Enhancement by Polarization Transfer XXI
7 8.5.1 The SPI Experiment The Two-Spin The INEPT Experiment () The Reverse INEPT Experiment Enhancement with Proton Detection Multi-Spin Sy~ 8.6 The DEPT Experiment From the One to the Two-Di 8.7 The Selective TOCSY Experiment NOESYand I 8.8 The One-Dimensional INADEQUATE )0.3 Experimental Experiment Applications. Exercises Exercises Bibliography for Chapter )0.5 Bibliography 9 Two-Dimensional NMR Spectroscopy Dynamic Nl 9.1 Introduction Introduction. 9.2 The Two-Dimensional NMR Experiment Quantitative ' Preparation, Evolution and Mixing, Complete Lin Data Acquisition The Coalesce Graphical Representation the Corresp Two-Dimensional ]-Resolved Activation Pa NMR Spectroscopy The Arrhenil Heteronuclear Two-Dimensional The Free Ent I-Resolved NMR Spectroscopy Estimating th Homonuclear Two-Dimensional Rate Constar ]-Resolved NMR Spectroscopy with Interme 9.4 Two-Dimensional Correlated Intermolecul; NMR Spectroscopy U.3 Applications Two-Dimensional Heteronuclear Rotation abo (C,H)-Correlated NMR Spectroscopy C(sp 3 )-C(sp (HETCOR or C,H-COSY) C( sp 2 )-C( sp Two-Dimensional Homo nuclear C(sp 2 )-C(sp (H,H)-Correlated NMR Spectroscopy Rotation abc (H,H-COSY; Long-Range COSY) Inversion at Reverse Two-Dimensional Ring Inversi1 Heteronuclear (H,C)-Correlated Valence Taut NMR Spectroscopy (HSQC; HMQC) Keto-Enol1l The Gradient-Selected Intermolecul (gs-)hmbc Experiment Reactions a The TOCSY Experiment Exercises Two-Dimensional Exchange ll.4 Bibliograph~ NMR Spectroscopy: The Experiments NOESY ROESY and EXSY Synthetic I 9.5 The Two-Dimensional INADEQUATE 12.1 Introductio11 Experiment The Tacticit: 9.6 Summary of Chapters 8 and Polymerizati Exercises Copolymers 9.7 Bibliography for Chapter Solid-State I Exercises.. 10 The Nuclear Overhauser Effect Bibliograph 10.1 Introduction Theoretical Background XXII
8 The Two-Spin System Enhancement Factors Multi-Spin Systems ]0.2.3 From the One-Dimensional to the Two-Dimensional Experiments, NOESY and ROESY Experimental Aspects Applications Exercises Bibliography for Chapter u U.1 U U Dynamic NMR Spectroscopy (DNMR).. Introduction Quantitative Calculations.... Complete Line-shape Analysis... :.... The Coalescence Temperature T c and the Corresponding Rate Constant kc..... Activation Parameters.... The Arrhenius Activation Energy EA..... The Free Enthalpy of Activation llg..... Estimating the Limits of Error.... Rate Constants in Reactions with Intermediate Stages Intermolecular Exchange Processes..... Applications..... Rotation about CC Single Bonds.... C(sp3)-C(sp 3 ) Bonds.... C(sp 2 )-C(sp 3 ) Bonds.... C(sp 2 )-C(sp 2 ) Bonds Rotation about a Partial Double Bond..... Inversion at Nitrogen and Phosphorus Atoms.. Ring Inversion.... Valence Tautomerism Keto-Enol Tautomerism.... Intermolecular Proton Exchange.... Reactions and Equilibration Processes.... Exercises.... Bibliography for Chapter U U.6 Synthetic Polymers..... Introduction.... The Tacticity of Polymers..... Polymerization of Dienes Copolymers Solid-State NMR Spectroscopy of Polymers... Exercises.... Bibliography for Chapter XXIII
![1 0.2.1 J().2.2 J(J.2.3 ]0.2.4 J0.3 J0.4 10.5 11 11.1 11.2 J 1.2.1 11.2.2 11.2.3 J1.2.3.1 11.2.3.2 11.2.3.3 11.2.4 11.2.5 11.3 11.3.1 11.3.1.1 11.3.1.2 11.3.1.3 11.3.2!1.3.3 11.3.4 11.. 5 11.3.6 11.3.7 11.](/docs-images/73/69409747/images/9-0.jpg "3.8 11.4 The Two-Spin System.......... Enhancement Factors............. Multi-Spin Systems..... From the One-Dimensional to the Two-Dimensional Experiments, NOESY and ROESY...... Experimental Aspects.")
9 J().2.2 J(J.2.3 ]0.2.4 J0.3 J J J ! The Two-Spin System Enhancement Factors Multi-Spin Systems..... From the One-Dimensional to the Two-Dimensional Experiments, NOESY and ROESY Experimental Aspects Applications... Exercises Bibliography for Chapter Dynamic NMR Spectroscopy (DNMR).. Introduction.... Quantitative Calculations ,.. Complete Line-shape Analysis.... The Coalescence Temperature T c and the Corresponding Rate Constant kc.... Activation Parameters The Arrhenius Activation Energy EA The Free Enthalpy of Activation tlg.... Estimating the Limits of Error.... Rate Constants in Reactions with Intermediate Stages Intermolecular Exchange Processes Applications Rotation about CC Single Bonds..... C(sp3) -C(sp3) Bonds C(sp 2 )-C(sp3) Bonds C(sp2)-C(sp 2 ) Bonds..... Rotation about a Partial Double Bond.... Inve r i n at itrogen and Phosphoru Atom.. Ring fnver ion Valenc Tautomerism Keto-Enol Tautomerism Intermolecular Pro ton Exchange Reaction and quilibrati n Processes Exercises Bibliography for Chapter U U.6 Synthetic Polymers.... Introduction The Tacticity of Polymers Polymerization ofdienes op lyn1er Soljd- tate NMR Spectroscopy of P Jyo1e r... ~ xercises Bibliography for Chapter XXIII
10 L3.2.J XXIV NMR Spectroscopy in Biochemistry and Medicine Introduction Elucidating Reaction Pathways in Biochemistry 355 Syntheses using Singly 13C-Labeled Precursors 356 Low Levels of J3C Enrichment High Levels of 13C Enrichment Syntheses using Doubly 13 C-Labeled Precursors 358 Biopolymers Peptides and Proteins Sequence Analysis The Three-Dimensional Structure of Proteins Polynucleotides Oligosaccharides and Polysaccharides Saturation Transfer Difference NMR Spectroscopy (STD) Exercises Bibliography for Chapter In vivo NMR Spectroscopy in Biochemistry and Medicine Introduction High-Resolution in vivo NMR Spectroscopy The Problem and its Solution lp NMR Experiments H and 13 C NMR Experiments Magnetic Resonance Tomography Basic Principles and Experimental Considerations Applications Magnetic Resonance Spectroscopy, 1 H MRS Exercises Bibliography for Chapter Solutions Subject Index Index of Compounds The Ph~ ofnmf 1.1 Introducti~ In 1946 two research gr and M. E. Packard and th R.V. Pound, independen nance signals for the first awarded the Nobel Prize 1 Since then nuclear magn has developed into an i1 chemists, physicists, anc During the first three deca ments relied on one-dim gives spectra having just being used to display the 1 two-dimensional NMR e> the start of a new era in l by these methods have being displayed in the tt even become possible to more dimensions, althoug techniques. The importa troscopy now occupies Nobel Prize for Chemistr to K. Wi.ithrich, and of t to P. Lauterbur and P. M on NMR methods in ch The new techniques tha years show that develop1 far from coming to an em This book aims to exr cially, NMR spectroscoj important of all spectrosc The main field of appli determining the structure mation for this is obtaint preting high-resolution r low viscosity (or in some niques and instruments tt years). In this book we w Basic One- and Two-Dimensi' Copyright 2011 WILEY-VC ISBN
Basic One- and Two-Dimensional NMR Spectroscopy
Horst Friebolin Basic One- and Two-Dimensional NMR Spectroscopy Third Revised Edition Translated by Jack K. Becconsall WILEY-VCH Weinheim New York Chichester Brisbane Singapore Toronto Contents XV 1 The
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