Modern NMR spectroscopy: a guide for chemists
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| Main Authors: | , |
|---|---|
| Format: | Book |
| Language: | English |
| Published: |
Oxford u.a.
Oxford Univ. Press
1993
|
| Edition: | 2. ed. |
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Physical Description: | XIV, 314 S. zahlr. graph. Darst. |
| ISBN: | 0198555679 |
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Record in the Search Index
| _version_ | 1804122670026981376 |
|---|---|
| adam_text | CONTENTS I 10 10 11 11 13 14 15 17 19 19 21 23 24 24 26 28 30 30 33 33
33 35 36 38 39 41 43 45 46 49 52 52 53 2. SPIN DECOUPLING AND DIFFERENCE
SPECTROSCOPY 56 2.1. INTRODUCTION 56 2.2. PRINCIPLES 56 2.3. GATED
DECOUPLING 57 INTRODUCTION 1. THE ONE-PULSE EXPERIMENT 1.1. INTRODUCTION
1.2. PRINCIPLES OF NUCLEAR MAGNETIC RESONANCE 1.2.1. MAGNETIZATION AND
PRECESSION 1.2.2. EFFECTS OF PULSES 1.2.3. THE ROTATING FRAME OF
REFERENCE 1.2.4. FREE INDUCTION DECAY 1.2.5. STIMULATION OF REAL SPIN
SYSTEMS 1.2.6. FOURIER TRANSFORMATION PHASING 1.2.7. RELAXATION 1.2.8.
SIGNAL-TO-NOISE RATIO AND SIGNAL AVERAGING 1.3. SAMPLING AND COMPUTING
CONSIDERATIONS 1.3.1. DIGITIZATION 1.3.2. QUADRATURE DETECTION 1.3.3.
DIGITAL RESOLUTION ZERO FILLING 1.3.4. SENSITIVITY AND RESOLUTION
ENHANCEMENT 1.3.5. SIGNAL INTENSITY IN FT SPECTRA 1.4. EXPERIMENTAL
CONSIDERATIONS 1.4.1. PULSE WIDTHS 1.4.2. PHASE CYCLING 1.4.3. DYNAMIC
RANGE AND MEMORY OVERFLOW 1.4.4. SPECTROMETER PERFORMANCE 1.4.5.
FIELD/FREQUENCY LOCK 1.4.6. SAMPLE PREPARATION 1.4.7. ROUTINE 1 H
SPECTRA 1.4.8. INTEGRATION 1.4.9. 13 C SPECTRA 1.4.10. LESS-RECEPTIVE
NUCLEI 1.5. SUMMARY AND CHEMICAL CONSEQUENCES 1.5.1. PULSE SEQUENCE
CONVENTIONS 1.5.2. SUMMARY 2.4. DIFFERENCE SPECTROSCOPY 57 2.5.
EXPERIMENTAL CONSIDERATIONS 60 2.5.1. GENERAL 60 2.5.2. SUPPRESSION OF
BLOCH-SIEGERT SHIFTS 61 2.6. SUMMARY AND CHEMICAL CONSEQUENCES 62 3.
MULTIPLE-PULSE EXPERIMENTS 63 3.1. INTRODUCTION 63 3.2. INVERSION
RECOVERY 63 3.3. SPIN-ECHOES AND TRANSVERSE RELAXATION 67 3.3.1. SIMPLE
ECHOES 67 3.3.2. J -MODULATION 71 3.3.3. THE EFFECT OF HOMONUCLEAR
COUPLING 77 3.4. POPULATION TRANSFER 78 3.5. COMBINING PULSE SEQUENCES
83 3.5.1. NET SELECTIVE POLARIZATION TRANSFER 83 3.5.2. SELECTIVE
POLARIZATION TRANSFER USING HARD PULSES 84 3.5.3. NON-SELECTIVE
POLARIZATION TRANSFER * INEPT 86 3.5.4. INVERSE INEPT 88 3.5.5.
REFOCUSED INEPT 89 3.6. EXPERIMENTAL CONSIDERATIONS 90 3.6.1. PULSE
WIDTH CALIBRATION 90 3.6.2. SELECTIVE, COMPOSITE, AND SHAPED PULSES 91
3.6.3. SPECTROMETER DESIGN 93 3.7. SUMMARY AND CHEMICAL CONSEQUENCES 94
4. THE SECOND DIMENSION 97 4.1. INTRODUCTION 97 4.1.1. A BASIC
TWO-DIMENSIONAL SEQUENCE 98 4.1.2. SOME PROPERTIES OF THE SECOND
DIMENSION 102 4.2. HETERONUCLEAR CHEMICAL SHIFT CORRELATION 104 4.2.1.
REMOVING HETERONUCLEAR COUPLING 104 4.2.2. REMOVING HOMONUCLEAR COUPLING
107 4.2.3. INVERSE-DETECTED SPECTRA * HMQC 110 4.3. HOMONUCLEAR SHIFT
CORRELATION * : COSY 113 4.3.1. BASIC SEQUENCE 114 4.3.2. VARIATIONS ON
COSY 117 4.3.3. SYMMETRIZATION 118 4.4. MULTIPLE QUANTUM COHERENCE *
INADEQUATE 119 4.5. SPIN-LOCKED SEQUENCES * TOCSY 122 4.6. DESIGNING NEW
SEQUENCES 123 4.6.1. SOLVENT-SUPPRESSED TWO-DIMENSIONAL SPECTROSCOPY 124
4.6.2. MULTIPLE-QUANTUM FILTERS 124 4.6.3. RELAY SEQUENCES 125 4.6.4.
THREE-DIMENSIONAL NMR 126 EXPERIMENTAL CONSIDERATIONS 127 4.7.1.
SPECTRAL WIDTH IN F I 127 4.7.2. DIGITAL RESOLUTION AND SPEED OF
ACQUISITION 128 4.7.3. PHASE CYCLING 130 4.7.4. SHIMMING 130 4.7.5.
PULSE WIDTHS 130 4.7.6. APODIZATION AND PHASING 131 4.7.7. THE ART OF
CONTOUR PLOTS 132 SUMMARY AND CHEMICAL CONSEQUENCES 133 CONNECTIONS
THROUGH BONDS 136 1. STRATEGY AND TACTICS 136 5.1.1. DEFINING THE
PROBLEM 136 5.1.2. ENTRY POINTS 138 5.1.3. CONNECTING FRAGMENTS 140 2.
MAKING HOMONUCLEAR CONNECTIONS 141 5.2.1. WHICH APPROACH? 141 WHICH COSY
APPROACH? 142 5.2.2. INTERPRETING 1 H COSY SPECTRA 143 5.2.3. OTHER
ABUNDANT SPINS 147 5.2.4. BIOSYNTHESIS AND MECHANISM USING 13 C COSY 148
5.2.5. DILUTE SPINS * INADEQUATE 150 3. MAKING HETERONUCLEAR CONNECTIONS
153 CONNECTIONS THROUGH SPACE 160 1. INTRODUCTION 160 2. THEORY 161
6.2.1. RELAXATION IN A TWO-SPIN SYSTEM 161 6.2.2. THE NOE IN A TWO-SPIN
SYSTEM 164 STEADY STATE NOES 164 TRANSIENT NOES 166 TWO-DIMENSIONAL NOES
* NOESY AND ROESY 167 6.2.3. SYSTEMS WITH THREE PROTONS 169 THE EFFECT
OF DISTANCE 169 THE EFFECT OF CORRELATION TIME 173 6.2.4. HETERONUCLEAR
MULTI-SPIN SYSTEMS 174 6.2.5. NOE DIFFERENCE SPECTROSCOPY 175 3. SUMMARY
AND CHEMICAL CONSEQUENCES 176 4. EXPERIMENTAL CONSIDERATIONS 177 6.4.1.
RELAXATION AND THE ROUTINE 13 C SPECTRUM 177 6.4.2. MEASURING RELAXATION
RATES 179 INVERSION RECOVERY 179 SATURATION RECOVERY 180 PROGRESSIVE
SATURATION 181 6.4.3. OPTIMIZING NOE DIFFERENCE SPECTRA 181 MAXIMIZING
ENHANCEMENTS 182 MAXIMIZING FREQUENCY SELECTIVITY 183 ACQUISITION
STRATEGIES 185 MINIMIZING SUBTRACTION ARTIFACTS 186 TRANSIENT AND
KINETIC NOES 186 HETERONUCLEAR NOES 187 6.4.4. OPTIMIZING NOESY SPECTRA
187 6.5. APPLICATIONS 188 6.5.1. SPECTROSCOPIC ASSIGNMENTS 188 6.5.2.
STRUCTURE DETERMINATIONS 193 6.5.3. CONFORMATIONAL STUDIES 197
VINBLASTINE 198 CONFORMATIONAL EQUILIBRIA OF ENOL ETHERS 200 PEPTIDES,
PROTEINS, AND NUCLEIC ACIDS 201 6.5.4. MOTION AND MOBILITY 201 7.
CONNECTIONS THROUGH CHEMICAL EXCHANGE 205 7.1. INTRODUCTION 205 7.2.
SPECTROSCOPIC TIMESCALES 205 7.2.1. FAST AND SLOW CHEMICAL EXCHANGE 205
UV AND IR TIMESCALES 207 7.2.2. LIFETIMES AND LINEWIDTHS 208 7.2.3. THE
J TIMESCALE 211 7.2.4. CHEMICAL SHIFT ANISOTROPY 214 7.2.5. THE R 1 AND
NOE TIMESCALE 215 7.2.6. CHEMICAL CONSEQUENCES 216 EFFECTS OF EXCHANGE
PROCESSES ON SPECTRA 216 CONTROLLING EXCHANGEABLE PROTONS 220 7.3.
TRANSFER OF SATURATION 222 7.3.1. THEORY 222 7.3.2. EXPERIMENTAL
CONSIDERATIONS 223 7.3.3. TRANSFERRED NOES 225 7.4. INVESTIGATING
EQUILIBRIUM PROCESSES 226 7.4.1. TRANSFER OF SATURATION OR MAGNETIZATION
227 7.4.2. EXCHANGE BROADENING AND SPIN-ECHOES 231 8. EDITING 235 8.1.
INTRODUCTION 235 8.2. BROADBAND DECOUPLING 236 8.2.1. HETERONUCLEAR
DECOUPLING 236 8.2.2. HOMONUCLEAR DECOUPLING: TWO-DIMENSIONAL J
-SPECTROSCOPY 238 8.3. SUPPRESSING BROAD LINES 243 8.3.1. MANIPULATION
OF THE FID 243 8.3.2. SPIN-ECHOES 244 SPIN-ECHO DECOUPLING DIFFERENCE
246 8.3.3. SELECTIVE SATURATION OF THE BROAD COMPONENT 246 8.4. SOLVENT
SUPPRESSION 247 8.4.1. SELECTIVE SATURATION 247 8.4.2. SELECTIVE
RELAXATION 248 8.4.3. SELECTIVE EXCITATION AND DETECTION 249 8.4.4.
SUMMARY OF SOLVENT SUPPRESSION 252 8.5. SUB-SPECTRA 253 8.5.1.
IDENTIFYING AND SEPARATING X H N SIGNALS 253 DEPT 254 COMPARISON OF
EDITING METHODS 256 EXTENSION TO SPECIAL CASES AND OTHER SYSTEMS 257
8.5.2. EDITING 1 H SPECTRA USING X-SPINS 257 9. SOLIDS 260 9.1.
INTRODUCTION 260 9.2. LINE BROADENING FOR SPIN-1/2 SAMPLES 260 9.2.1.
DIPOLAR BROADENING 261 9.2.2. SPIN-SPIN RELAXATION 262 9.2.3. CHEMICAL
SHIFT ANISOTROPY 263 9.3. LINE NARROWING 263 9.3.1. MAGIC ANGLE SPINNING
264 9.3.2. DIPOLAR DECOUPLING 265 COMBINED MAS AND DIPOLAR DECOUPLING
265 9.3.3. MULTIPLE-PULSE LINE NARROWING 266 9.4. CROSS POLARIZATION 267
9.4.1 CROSS POLARIZATION AND RELAXATION 269 9.5. SPECTRAL IMPROVEMENT
AND EDITING 270 9.6 TWO-DIMENSIONAL EXPERIMENTS ON SOLIDS 270 9.7.
NUCLEI WITH SPIN 1/2 273 9.8. EXPERIMENTAL CONSIDERATIONS 275 9.9.
CHEMICAL APPLICATIONS 278 9.10. SUMMARY AND CONCLUSIONS 282 10. SUCROSE
OCTA-ACETATE: A CASE HISTORY 287 10.1. INTRODUCTION 287 10.1.1. THE
CHOICE OF MOLECULE 287 10.1.2. OBJECTIVES 288 10.2. ONE-DIMENSIONAL
SPECTRA 288 10.2.1. 1 H SPECTRA 288 CHLOROFORM SOLUTION 288 BENZENE
TITRATION 289 DECOUPLING DIFFERENCE SPECTRA 290 10.2.2. 13 C SPECTRA 291
10.3. TWO-DIMENSIONAL SPECTRA 292 10.3.1. COSY 292 10.3.2. 1 H- 13 C
CHEMICAL SHIFT CORRELATION 294 10.4. NOE DIFFERENCE SPECTRA 295 10.5.
OTHER EXPERIMENTS 10.6. SUMMARY OF RESULTS 10.7. CONCLUSION 299 299 300
APPENDIX. SYMMETRY, NON-EQUIVALENCE, AND RESTRICTED ROTATION 303 A.L.
THE INFLUENCE OF CHIRALITY 303 A.2. THE SUBSTITUTION TEST FOR
NON-EQUIVALENCE 305 A.3. RESTRICTED ROTATION 306 INDEX 309
|
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| spelling | Sanders, Jeremy K. Verfasser aut Modern NMR spectroscopy a guide for chemists Jeremy K. M. Sanders ; Brian K. Hunter 2. ed. Oxford u.a. Oxford Univ. Press 1993 XIV, 314 S. zahlr. graph. Darst. txt rdacontent n rdamedia nc rdacarrier Ackermann-Gemeinde (DE-588)39042-2 gnd rswk-swf Nuclear magnetic resonance spectroscopy NMR gtt Spectroscopie de la résonance magnétique nucléaire NMR-Spektroskopie (DE-588)4075421-2 gnd rswk-swf 1\p (DE-588)4123623-3 Lehrbuch gnd-content NMR-Spektroskopie (DE-588)4075421-2 s 2\p DE-604 Ackermann-Gemeinde (DE-588)39042-2 b 3\p DE-604 Hunter, Brian K. Verfasser aut OEBV Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=005465826&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis 1\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 2\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 3\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk |
| spellingShingle | Sanders, Jeremy K. Hunter, Brian K. Modern NMR spectroscopy a guide for chemists Ackermann-Gemeinde (DE-588)39042-2 gnd Nuclear magnetic resonance spectroscopy NMR gtt Spectroscopie de la résonance magnétique nucléaire NMR-Spektroskopie (DE-588)4075421-2 gnd |
| subject_GND | (DE-588)39042-2 (DE-588)4075421-2 (DE-588)4123623-3 |
| title | Modern NMR spectroscopy a guide for chemists |
| title_auth | Modern NMR spectroscopy a guide for chemists |
| title_exact_search | Modern NMR spectroscopy a guide for chemists |
| title_full | Modern NMR spectroscopy a guide for chemists Jeremy K. M. Sanders ; Brian K. Hunter |
| title_fullStr | Modern NMR spectroscopy a guide for chemists Jeremy K. M. Sanders ; Brian K. Hunter |
| title_full_unstemmed | Modern NMR spectroscopy a guide for chemists Jeremy K. M. Sanders ; Brian K. Hunter |
| title_short | Modern NMR spectroscopy |
| title_sort | modern nmr spectroscopy a guide for chemists |
| title_sub | a guide for chemists |
| topic | Ackermann-Gemeinde (DE-588)39042-2 gnd Nuclear magnetic resonance spectroscopy NMR gtt Spectroscopie de la résonance magnétique nucléaire NMR-Spektroskopie (DE-588)4075421-2 gnd |
| topic_facet | Ackermann-Gemeinde Nuclear magnetic resonance spectroscopy NMR Spectroscopie de la résonance magnétique nucléaire NMR-Spektroskopie Lehrbuch |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=005465826&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
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