One and two dimensional NMR spectroscopy:
Gespeichert in:
| 1. Verfasser: | |
|---|---|
| Format: | Buch |
| Sprache: | German |
| Veröffentlicht: |
Amsterdam [u.a.]
Elsevier
1989
|
| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis |
| Beschreibung: | Literaturangaben |
| Beschreibung: | XIX, 578 S. Ill., graph. Darst. |
| ISBN: | 0444873163 |
Internformat
MARC
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Datensatz im Suchindex
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| adam_text | ONE AND TWO
DIMENSIONAL NMR
SPECTROSCOPY
Atta-ur-Rahman
HEJ Research Institute of Chemistry,
University of Karachi,
Karachi 32, Pakistan
ELSEVIER
Amsterdam — Oxford — New York — Tokyo 1989
IX
CONTENTS
Chapter-l
1 BASIC PRINCIPLES OF MODERN NMR SPECTROSCOPY
1 1 Introduction
1 2 Some Fundamental Considerations in NMR Spectroscopy
121 Instrumentation
12 1 1 The Magnet
1212 The Probe
1 2 13 Probe Tuning
1214 Shimming
1215 Deuterium Lock
122 Creating a Signal
1 23 Pulse NMR
124 Data Acquisition and Storage
1241 The Dynamic Range Problem
125 Digital Resolution
12 6 Quadrature Detection
1261 Peak Folding
127 Fourier Transformation
128 Signal-to-Noise Ratio
129 Manipulating the Spectrum - Window Functions
1291 Sensitivity Enhancement
1292 Resolution Enhancement
1 2 10 Rotating Frame of Reference
1 2 10 1 Pulse Angle
1 2 10 2 Rotation of Vectors
1 2 11 Phase Cycling
1 2 11 1 Phase Cycling and Coherence Pathways
1 2 12 Pulse Widths
1 2 12 1 Composite Pulses
1 2 13 Time Proportional Phase Increment (TPPI)
12 14 Tailored Suppression and Excitation -
Solvent Suppression Techniques
1 2 14 1 Presaturation
X
1 2 142 Tailored Excitation Method 44
1 2 143 Jump and Return Method 44
12 14 4 The Inversion Recovery Method 45
1 2 14 5 Solvent Suppression by Paramagnetic Reagents 46
1 2 14 6 Selective Excitation by DANTE (Delays
Alternating with Nutation for
Tailored Excitation) 46
1 2 14 7 Improvements in Instrumentation Design 48
(a) Probehead Design 48
(b) Offset Equivalence of Transmitter
and Decoupler Channels 48
(c) Fast Switching of Decoupler Power 48
1 2 15 Nuclear Overhauser Enhancement (NOE) 49
12 16 Theoretical Approaches to Pulsed NMR 49
12 16 1 Bloch s Semi-classical Approach 49
12 162 Density Matrix Approach 50
1 2 163 Product Operator Approach 50
12 17 Effect of a Pulse on the Nucleus 54
1 2 18 Coherence Transfer 57
12 18 1 Homonuclear Coherence Transfer 57
12 18 2 Heteronuclear Coherence Transfer 62
12 19 Multiple Quantum Filters 66
1 220 Other Selective Detection Techniques 68
1 220 1 p-Spin Filtering 68
12 20 2 z-Filters 71
Chapter-2
2 SPIN-ECHO AND POLARISATION TRANSFER 77
2 1 Spin-Echo Formation in Homonuclear and Heteronuclear
Systems 77
211 Spin-Echo Production in Heteronuclear Systems 77
2111 18(P Pulse Applied Simultaneously to
Nuclei A and X 11
2 1 12 18(f Pulse Applied Selectively to
Partner Nucleus X 80
2 12 Spin-Echo Production in Homonuclear
Systems (or Heteronuclear Systems with
XI
Non-Selective Application of Pulses) 80
2 12 1 18(f Pulse Applied Simultaneously
to Nuclei A and X 80
2 13 Attached Proton Test (APT), Gated Spin-Echo
(GASPE) or Spin-Echo Fourier Transform
(SEFT) Measurements 82
2 13 1 Escort Editing of APT Spectra 93
2 2 Cross-polarisation 94
221 Selective Population Transfer 95
222 Non-Selective Polarisation Transfer 100
2221 Insensitive Nuclei Enhanced by
Polarisation- Transfer (INEPT) 100
2 22 1 1 Refocussed INEPT 105
2 22 12 INEPT+ 107
22 2 13 Reverse INEPT 107
223 Semi-Selective Excitation for Polarisation
Transfer (SESET) 107
2 23 1 SESET-RELAY 109
224 Distortionless Enhancement by Polarisation
Transfer (DEPT) and Related Experiments 111
2241 DEPT 111
22 411 Anomalies in Polarisation Transfer
Experiments 116
(a) Intensity Anomalies 116
(b) Multiplet Anomalies 116
(c) Phase Anomalies 116
(d) Incomplete Separation of Subspectra 116
2 2 42 DEPT+ 116
2 2 43 DEPT++ 116
2244 DEPTGL 117
22 4 5 MODEPT 118
22 4 6 Universal Polarisation Transfer (UPT) 118
22 4 7 Phase Oscillation to Maximise
Editing (POMMIE) 118
2248 Reverse DEPT 118
22 4 9 Subspectral Editing Using a
Multiple Quantum Trap (SEMUT) 122
22 491 SEMUT GL 123
XII
23 Problems 125
2 4 Solutions to Problems 133
Chapter-3
3 CARBON-CARBON CONNECTIVITY-ID INADEQUATE 141
SPECTRA
3 1 Introduction 141
32 One-dimensional INADEQUATE 13C-NMR Spectra 143
32 1 Factors Affecting the Intensity of the
13C Satellite Signals 152
3 22 Some Practical Suggestions 153
3 23 SEMUT Editing of INADEQUATE
Spectra (SEMINA) 154
32 4 INEPT-INADEQUATE 157
32 5 DEPT-INADEQUATE 157
32 6 INADEQUATE Sensitivity Improvement by
Proton Indirect Detection (INSIPID) 159
32 7 Saturation INADEQUATE 159
32 8 Double-Quantum Transitions for
Finding Unresolved Lines (DOUBTFUL) 161
Chapter-4
4 THE NUCLEAR OVERHAUSER EFFECT 167
4 1 Introduction 167
42 Relaxation Pathways 168
42 1 Spin-Lattice Relaxation 168
422 Other Relaxation Mechanisms 168
43 How nOe Occurs 169
4 4 Other Factors Governing Relaxation and nOe 174
4 5 Interauclear Distance and nOe 178
451 Internuclear Distances in Two-Spin
Systems 179
XIII
4 52 Three-Spin Systems
4 52 1 Linear Arrangement
4 52 1 1 Three-Spin Effect
4 52 2 Non-Linear Arrangement
4 6 Heteronuclear nOe
4 7 NOE Difference Spectra
471 Some Practical Examples of nOe Difference
Spectroscopy
4 8 Problems
4 9 Solutions to Problems
Chapter-5
5 TWO-DIMENSIONAL NMR SPECTROSCOPY- 203
BASIC PRINCIPLES
Chapter-6
6 HETERONUCLEAR 2D J-RESOLVED SPECTROSCOPY 217
6 1 The Gated Decoupler Method 222
62 The Refocussed Fold-over Corrected (RE-FOCSY)
Gated Decoupler Method 225
63 The Spin-Flip Method 226
6 4 The Selective Spin-Flip Method 226
6 5 The Semi-Selective Spin-Flip Method 230
6 6 Indirect J-Spectroscopy with Selective Spin-Flip 234
6 7 Heteronuclear 2D J-resolved Spectra with
Polarisation Transfer 235
6 8 Heteronuclear 2D J-resolved Spectra with Driven Pulses 236
6 9 Problems 237
6 10 Solutions to Problems 239
XIV
Chapter-7
7 HOMONUCLEAR 2D J-RESOLVED SPECTROSCOPY 245
7 1 Double Resonance in 2D J-Resolved Spectra 255
7 2 Constant Time 2D J-Resolved Spectra 255
73 Absorption mode 2D J-Resolved Spectra 257
7 4 Differentiation of Homonuclear Multiplets by
Indirect 2D J-Resolved Spectroscopy 258
7 5 Problems 260
7 6 Solutions to Problems 264
Chapter 8
8 HOMONUCLEAR 2D SHIFT CORRELATED 269
SPECTROSCOPY
8 1 COSY Spectra 269
811 Introduction 269
812 The Nuts and Bolts of COSY 272
8121 Magnetization Transfer 272
8 1 22 Phase Cycling 274
8 13 The Birth of a COSY Spectrum 277
814 Intensity of Cross-Peaks 281
815 Digital Resolution in COSY 281
816 Other Practical Considerations in COSY 282
817 Some Examples of COSY Spectra 284
818 Improvements in COSY Spectra 287
8181 Elimination of Artifact Axial Peaks
Parallel to vi from COSY Spectra 287
8182 Noise in COSY Spectra 289
8 1 83 Quad Detection and Suppressing Quad
Images in COSY Spectra 291
819 Phase-Sensitive COSY Spectra 293
8191 Pure-Phase 2D Spectra by Cosine
Transformation with respect to ti 299
8 1 92 Coupling Constants from Phase-Sensitive
COSY Spectra 299
XV
8 1 10 COSY by Echo or Anti-echo Selection 305
8 1 11 Basic Peakshapes in 2D Spectra 306
8 1 11 1 Pure 2D Absorption Peakshape 306
8 1 112 Pure 2D Dispersion Peakshape 306
8 1 113 Mixed Absorption-Dispersion Peakshape
(Phase-twisted Peakshape) 308
8 1 11 4 Absolute Value Peakshape 308
8 1 12 Shaping Functions in 2D Spectra 309
8 1 13 Folding of Signals in COSY Spectra 313
8 1 14 Symmetrization 313
8 1 15 Coherence Transfer Pathways in COSY 315
82 Modifications in COSY Spectra 317
82 1 COSY-45 Spectra 317
82 1 1 Pattern Recognition 321
8 2 12 Signs of Coupling Constants 321
8 2 13 COSY-45 Spectra with Decoupling
in vi Dimension 323
822 COSY Optimized for Long Range Couplings
(DELAYED COSY) 327
823 Super COSY 328
824 Exclusive Correlation Spectroscopy
(E COSY) 329
82 5 Homonuclear Relayed Coherence Transfer
(Relayed COSY or R COSY) 331
826 Homonuclear Chemical Shift Correlation
by Heteronuclear Relayed Coherence
Transfer (HERPECS) 335
827 Total Correlation Spectroscopy (TOCSY) 337
82 8 SECSY 341
82 9 z-Filtered SECSY Spectra 344
82 10 FOCSY Spectra 345
8 2 11 Super SECSY 346
82 12 Difference SECSY 347
8 2 13 vi -Decoupled SECSY Spectra 348
83 Problems 349
XVI
8 4 Solutions to Problems 352
Chapter-9
9 CHEMICAL SHIFT CORRELATION THROUGH 359
CROSS - RELAXATION AND EXCHANGE
9 1 Introduction 359
9 2 Nuclear Overhauser Enhancement Spectroscopy (NOESY) 360
921 Homonuclear Relayed NOESY 365
922 Heteronuclear Relayed NOESY 367
93 2D Chemical Exchange Spectra 369
93 1 Rate Constant by Accordion Spectroscopy -
Three-Dimensional NMR 371
9 4 CAMELSPIN OR ROESY (Rotating Frame Overhauser
Enhancement Spectroscopy) 373
9 5 Two-Dimensional Heteronuclear NOE
Spectroscopy (HOESY) 376
9 6 Combined COSY-NOESY Experiment (COCONOSY) 379
9 7 DQ NOESY 380
9 8 Problems 381
9 9 Solutions to Problems 384
Chapter-10
10 HETERONUCLEAR 2D-SHIFT CORRELATION 391
SPECTROSCOPY
10 1 Principles of Heteronuclear 2D Shift Correlation
Spectroscopy 391
10 2 Modifications of Heteronuclear 2D-Shift
Correlation Experiment 398
102 1 With Homonuclear vi Decoupling 398
1022 Long Range Heteronuclear Chemical Shift
Correlation using (TANGO) 399
1023 Improved Decoupling Modulation Procedures
XVII
in 2D Long-Range Heteronuclear Chemical
Shift Correlation Spectra 401
10 2 4 Correlation Spectroscopy via Long-Range
Coupling (COLOC) 404
102 5 1H-Detected Heteronuclear Multiple-Quantum
Coherence (HMQC) for Correlating Directly
Bonded ^-c Nuclei 406
10 2 6 Sensitivity Enhanced Detection of Heteronuclear
Multiple Bond Connectivity (HMBC) by 2D
Multiple-Quantum NMR 409
10 2 7 2D DEPT Heteronuclear Shift Correlation
Spectroscopy 412
103 Sensitivity of Heteronuclear Coherence Transfer
Experiments 414
10 4 Heteronuclear Relayed Coherence Transfer Spectroscopy
(or Heteronuclear Relayed COSY) 416
10 4 1 Low Pass J-Filtered 2D Heteronuclear Shift
Correlated Spectra 422
10 4 2 Relayed Coherence Transfer From a Heteronucleus
through Proton Spin Systems 423
10 43 Heteronuclear Relayed Coherence Transfer via
Hartmann-Hahn type Cross-Polarisation 423
10 5 Problems 427
10 6 Solutions to Problems 429
Chapter-11
11 CROSS POLARISATION IN THE ROTATING FRAME 435
11 1 Introduction 435
11 2 Homonuclear Hartmann-Hahn Spectroscopy (HOHAHA) 436
XVIII
Chapter-12
12 2D MULTIPLE-QUANTUM SPECTROSCOPY 447
12 1 Introduction 447
122 Multiple-Quantum Spectra of Two Spin Systems 450
12 2 1 Two Dimensional INADEQUATE 13C-NMR
Spectroscopy 450
12 211 Proton Monitored INADEQUATE
(INSIPID) 456
123 Multiple-Quantum Spectra of Three-Spin Systems 459
123 1 Double-Quantum Spectra of Three-Spin
Systems • 459
123 1 1 Linear Systems 459
(i) Signals due to Direct Connectivity 462
(ii) Magnetically Equivalent Nuclei 462
(Hi) Remote Nuclei 462
123 2 Triple-Quantum Spectra of Three-Spin Systems 463
123 2 1 Constant Time Double-Quantum Spectroscopy 466
12 4 Multiple-Quantum Spectra in Four-Spin Systems 467
12 5 Uniform Excitation of Multiple-Quantum Coherence 468
12 6 Multiple-Quantum Filtered COSY Spectra 470
12 7 Homonuclear Zero-Quantum Spectroscopy 475
12 7 1 Improved HZQC Method 478
12 7 2 SUCZESS 481
12 8 Problems 484
12 9 Solutions to Problems 487
Chapter-13
13 TACKLING THE STRUCTURE 493
13 1 Choice of Experiment 493
13 2 A Case Study • 495
(a) W JH-NMR Studies 496
(b) Homonuclear 2D J-Resolved Spectrum 499
XIX
(c) 2D Homonuclear Shift Correlated
Spectrum (COSY-45) 499
(d) DEPT Spectra 499
(e) 2D Heteronuclear Shift Correlated Experiment 503
(f) H,13C-COLOC 505
(g) NOESY and NOE Difference Spectra 507
(h) 2DINADEQUA TE Spectrum 510
Chapter-14
14 PRODUCT OPERATOR APPROACH TO 2D-NMR 511
SPECTROSCOPY
14 1 Scalar Coupling 514
142 Dipolar Coupling 518
143 Phase Cycling and Product Operators 521
Appendix-1 SOME TERMS, SYMBOLS AND ACRONYMS
USED IN NMR SPECTROSCOPY 527
Appendix-2 SUMMARY OF IMPORTANT 2D NMR
TECHNIQUES 537
Index 553
|
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| id | DE-604.BV004159929 |
| illustrated | Illustrated |
| indexdate | 2024-07-09T16:09:14Z |
| institution | BVB |
| isbn | 0444873163 |
| language | German |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-002594215 |
| oclc_num | 18990444 |
| open_access_boolean | |
| owner | DE-91G DE-BY-TUM DE-355 DE-BY-UBR DE-20 DE-83 DE-11 |
| owner_facet | DE-91G DE-BY-TUM DE-355 DE-BY-UBR DE-20 DE-83 DE-11 |
| physical | XIX, 578 S. Ill., graph. Darst. |
| publishDate | 1989 |
| publishDateSearch | 1989 |
| publishDateSort | 1989 |
| publisher | Elsevier |
| record_format | marc |
| spelling | Atta-ur-Rahman 1942- Verfasser (DE-588)111146356 aut One and two dimensional NMR spectroscopy Atta-ur-Rahman Amsterdam [u.a.] Elsevier 1989 XIX, 578 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Literaturangaben Nuclear magnetic resonance spectroscopy Zweidimensionale NMR-Spektroskopie (DE-588)4191219-6 gnd rswk-swf NMR-Spektroskopie (DE-588)4075421-2 gnd rswk-swf NMR-Spektroskopie (DE-588)4075421-2 s DE-604 Zweidimensionale NMR-Spektroskopie (DE-588)4191219-6 s HEBIS Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=002594215&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Atta-ur-Rahman 1942- One and two dimensional NMR spectroscopy Nuclear magnetic resonance spectroscopy Zweidimensionale NMR-Spektroskopie (DE-588)4191219-6 gnd NMR-Spektroskopie (DE-588)4075421-2 gnd |
| subject_GND | (DE-588)4191219-6 (DE-588)4075421-2 |
| title | One and two dimensional NMR spectroscopy |
| title_auth | One and two dimensional NMR spectroscopy |
| title_exact_search | One and two dimensional NMR spectroscopy |
| title_full | One and two dimensional NMR spectroscopy Atta-ur-Rahman |
| title_fullStr | One and two dimensional NMR spectroscopy Atta-ur-Rahman |
| title_full_unstemmed | One and two dimensional NMR spectroscopy Atta-ur-Rahman |
| title_short | One and two dimensional NMR spectroscopy |
| title_sort | one and two dimensional nmr spectroscopy |
| topic | Nuclear magnetic resonance spectroscopy Zweidimensionale NMR-Spektroskopie (DE-588)4191219-6 gnd NMR-Spektroskopie (DE-588)4075421-2 gnd |
| topic_facet | Nuclear magnetic resonance spectroscopy Zweidimensionale NMR-Spektroskopie NMR-Spektroskopie |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=002594215&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT attaurrahman oneandtwodimensionalnmrspectroscopy |