Basic one- and two-dimensional NMR spectroscopy:
Gespeichert in:
| 1. Verfasser: | |
|---|---|
| Format: | Buch |
| Sprache: | English |
| Veröffentlicht: |
Weinheim
Wiley-VCH
2011
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| Ausgabe: | 5., completely rev. and enlarged. ed. |
| Schlagworte: | |
| Online-Zugang: | Inhaltstext Inhaltsverzeichnis |
| Beschreibung: | XXIV, 418 S. Ill., graph. Darst. |
| ISBN: | 9783527327829 |
Internformat
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CONTENTS 1 THE PHYSICAL BASIS OF NMR SPECTROSCOPY 1 1.1 INTRODUCTION 1
1.2 NUCLEAR ANGULAR MOMENTUM AND MAGNETIC MOMENT 2 1.3 NUCLEI IN A
STATIC MAGNETIC FIELD 4 1.3.1 DIRECTIONAL QUANTIZATION 4 1.3.2 ENERGY OF
THE NUCLEI IN THE MAGNETIC FIELD. 4 1.3.3 POPULATIONS OF THE ENERGY
LEVELS 6 1.3.4 MACROSCOPIC MAGNETIZATION 6 1.4 BASIC PRINCIPLES OF THE
NMR EXPERIMENT 7 1.4.1 THE RESONANCE CONDITION 7 1.4.2 BASIC PRINCIPLE
OF THE NMR MEASUREMENT . 8 1.5 THE PULSED NMR METHOD 9 1.5.1 THE
PULSE 9 1.5.2 THE PULSE ANGLE 10 1.5.3 RELAXATION 13 1.5.4 THE TIME AND
FREQUENCY DOMAINS; THE FOURIER TRANSFORMATION 14 1.5.5 SPECTRUM
ACCUMULATION 16 1.5.6 THE PULSED NMR SPECTROMETER 18 1.6 SPECTRAL
PARAMETERS: A BRIEF SURVEY 22 1.6.1 THE CHEMICAL SHIFT 22 1.6.1.1
NUCLEAR SHIELDING 22 1.6.1.2 REFERENCE COMPOUNDS AND THE 5-SCALE 24
1.6.2 SPIN-SPIN COUPLING 26 1.6.2.1 THE INDIRECT SPIN-SPIN COUPLING 26
1.6.2.2 COUPLING TO ONE NEIGHBORING NUCLEUS (AX SPIN SYSTEM) 27 1.6.2.3
COUPLING TO TWO EQUIVALENT NEIGHBORING NUCLEI (AX 2 SPIN SYSTEM) 29
1.6.2.4 COUPLING TO THREE OR MORE EQUIVALENT NEIGHBORING NUCLEI (AX N
SPIN SYSTEM) 30 1.6.2. BIBLIOGRAFISCHE INFORMATIONEN
HTTP://D-NB.INFO/100402410X DIGITALISIERT DURCH 1.6.2.9 COUPLINGS
BETWEEN PROTONS AND OTHER NUCLEI; 13 C SATELLITE SPECTRA 33 1.6.3 THE
INTENSITIES OF THE RESONANCE SIGNALS 34 1.6.3.1 'H SIGNAL INTENSITIES 34
1.6.3.2 13 C SIGNAL INTENSITIES 35 1.6.4 SUMMARY 37 1.7 "OTHER" NUDIDES
38 1.7.1 NUCLIDES WITH SPIN/= 1/2 39 1.7.2 NUCLIDES WITH SPIN / 1/2 40
EXERCISES 41 1.8 BIBLIOGRAPHY FOR CHAPTER 1 41 2 THE CHEMICAL SHIFT 43
2.1 INTRODUCTION 43 2.1.1 INFLUENCE OF THE CHARGE DENSITY ON THE
SHIELDING 44 2.1.2 EFFECTS OF NEIGHBORING GROUPS 47 2.1.2.1 MAGNETIC
ANISOTROPY OF NEIGHBORING GROUPS . . 47 2.1.2.2 RING CURRENT EFFECTS 49
2.1.2.3 ELECTRIC FIELD EFFECTS 51 2.1.2.4 INTERMOLECULAR INTERACTIONS -
HYDROGEN BONDING AND SOLVENT EFFECTS 51 2.1.2.5 ISOTOPE EFFECTS 51 2.1.3
SUMMARY 52 2.2 1 H CHEMICAL SHIFTS OF ORGANIC COMPOUNDS . 53 2.2.1
ALKANES AND CYCLOALKANES 54 2.2.2 ALKENES 56 2.2.3 ARENES 56 2.2.4
ALKYNES 57 2.2.5 ALDEHYDES 58 2.2.6 OH,SH,NH 59 2.3 13 C CHEMICAL SHIFTS
OF ORGANIC COMPOUNDS . 60 2.3.1 ALKANES AND CYCLOALKANES 61 2.3.2
ALKENES 63 2.3. 3 INDIRECT SPIN-SPIN COUPLING 85 3.1 INTRODUCTION 85 3.2
H,H COUPLING CONSTANTS AND CHEMICAL STRUCTURE 87 3.2.1 GEMINAI COUPLINGS
2 7(H,H) 87 3.2.1.1 DEPENDENCE ON BOND ANGLE 87 3.2.1.2 SUBSTITUENT
EFFECTS 88 3.2.1.3 EFFECTS OF NEIGHBORING 7R-ELECTRONS 88 3.2.2 VICINAL
COUPLINGS -V(H,H) 89 3.2.2.1 DEPENDENCE ON THE DIHEDRAL ANGLE 90 3.2.2.2
SUBSTITUENT EFFECTS 94 3.2.3 H,H COUPLINGS IN AROMATIC COMPOUNDS 95
3.2.4 LONG-RANGE COUPLINGS 96 3.3 C,H COUPLING CONSTANTS AND CHEMICAL
STRUCTURE 97 3.3.1 C,H COUPLINGS THROUGH ONE BOND '7 (C,H) . 97
3.3.1.1 DEPENDENCE ON THE S-FRACTION 97 3.3.1.2 SUBSTITUENT EFFECTS 98
3.3.2 C,H COUPLINGS THROUGH TWO OR MORE BONDS. . . 99 3.3.2.1 GEMINAI
COUPLINGS (I. E. 2 7(C,H) IN H-C- L1 C) 99 3.3.2.2 VICINAL COUPLINGS
(I.E. V(C,H) IN H-C-C-'^C) 99 3.3.2.3 LONG-RANGE COUPLINGS 3 + "J(C,H)
100 3.3.3 C,H COUPLINGS IN BENZENE DERIVATIVES 100 3.4 C,C COUPLING
CONSTANTS AND CHEMICAL STRUCTURE 101 3.5 CORRELATIONS BETWEEN C,H AND
H,H COUPLING CONSTANTS 101 3.6 COUPLING MECHANISMS 1 03 3.6.1 THE
ELECTRON-NUCLEAR INTERACTION 103 3.6. 4.4 THREE-SPIN SYSTEMS 1 20 4.4. 1
THE AX 2 , AK 2 , AB 2 AND A 3 SPIN SYSTEMS 120 4.4.2 THE AMX AND ABX
SPIN SYSTEMS 121 4.5 FOUR-SPIN SYSTEMS 123 4.5.1 A 2 X 2 AND A 2 B 2
SPIN SYSTEMS 123 4.5.2 THE AA'XX' AND AA'BB' SPIN SYSTEMS 124 4.6
SPECTRUM SIMULATION AND ITERATION 125 4.7 ANALYSIS OF I3 C NMR SPECTRA 1
26 EXERCISES 127 4.8 BIBLIOGRAPHY FOR CHAPTER 4 127 5 DOUBLE RESONANCE
EXPERIMENTS 129 5.1 INTRODUCTION 129 5.2 SPIN DECOUPLING IN 1 H NMR
SPECTROSCOPY. . 130 5.2.1 SIMPLIFICATION OF SPECTRA BY SELECTIVE SPIN
DECOUPLING 130 5.2.2 SUPPRESSION OF A SOLVENT SIGNAL 132 5.3 SPIN
DECOUPLING IN U C NMR SPECTROSCOPY . 133 5.3.1 'H BROAD-BAND
DECOUPLING 133 5.3.2 THE GATED DECOUPLING EXPERIMENT 135 5.3.3 'H
OFF-RESONANCE DECOUPLING 136 5.3.4 SELECTIVE DECOUPLING IN 13 C 6.3.4 T\
MEASUREMENTS 160 6.3.5 CHEMICAL CHANGES TO THE SAMPLE 160 6.3.6 SOLVENT
AND TEMPERATURE EFFECTS AND SHIFT REAGENTS 161 6.4 COMPUTER-AIDED
ASSIGNMENT OF 13 C NMR SPECTRA 161 6.4. 1 SEARCHING FOR IDENTICAL OR
RELATED COMPOUNDS 161 6.4.2 SPECTRUM PREDICTION 162 EXERCISES 164 6.5
BIBLIOGRAPHY FOR CHAPTER 6 165 7 RELAXATION 167 7.1 INTRODUCTION 167 7.2
SPIN-LATTICE RELAXATION OF 13 C NUCLEI (TI) 168 7.2.1 RELAXATION
MECHANISMS 168 7.2.2 EXPERIMENTAL DETERMINATION OF T\; THE INVERSION
RECOVERY EXPERIMENT 170 7.2.3 RELATIONSHIPS BETWEEN T\ AND CHEMICAL
STRUCTURE 174 7.2.3.1 INFLUENCE OF PROTONS IN CH, CH 2 AND CH 3 GROUPS
174 7.2.3.2 INFLUENCE OF MOLECULAR SIZE 175 7.2.3.3 SEGMENTAL MOBILITIES
176 7.2.3.4 ANISOTROPY OF THE MOLECULAR MOBILITY 176 7.2.4 SUPPRESSION
OF THE WATER SIGNAL 177 7.3 SPIN-SPIN RELAXATION (T 2 ) 177 7.3.1
RELAXATION MECHANISMS 177 7.3.2 EXPERIMENTAL DETERMINATION OF 7V, TH
8.5.1 THE SPI EXPERIMENT 210 8.5.2 THE INEPT EXPERIMENT 213 8.5.3 THE
REVERSE INEPT EXPERIMENT WITH PROTON DETECTION 221 8.6 THE DEPT
EXPERIMENT 226 8.7 THE SELECTIVE TOCSY EXPERIMENT 230 8.8 THE
ONE-DIMENSIONAL INADEQUATE EXPERIMENT 233 EXERCISES 237 8.9 BIBLIOGRAPHY
FOR CHAPTER 8 237 9 TWO-DIMENSIONAL NMR SPECTROSCOPY . 239 9.1
INTRODUCTION 239 9.2 THE TWO-DIMENSIONAL NMR EXPERIMENT 240 9.2.1
PREPARATION, EVOLUTION AND MIXING, DATA ACQUISITION 240 9.2.2 GRAPHICAL
REPRESENTATION 244 9.3 TWO-DIMENSIONAL J-RESOLVED NMR SPECTROSCOPY 245
9.3.1 HETERONUCLEAR TWO-DIMENSIONAL /-RESOLVED NMR SPECTROSCOPY 245
9.3.2 HOMONUCLEAR TWO-DIMENSIONAL J-RESOLVED NMR SPECTROSCOPY 249 9.4
TWO-DIMENSIONAL CORRELATED NMR SPECTROSCOPY 254 9.4.1 TWO-DIMENSIONAL
HETERONUCLEAR (C,H)-CORRELATED NMR SPECTROSCOPY (HETCOR OR CH-COSY) 255
9.4.2 TWO-DIMENSIONAL HOMONUCLEAR (H,H)-CORRELATED NMR SPECTROSCOPY
(H,H-COSY; LONG-RANGE COSY) 263 9.4.3 REVERSE TWO-DIMENSIONAL
HETERONUCLEAR (H,C)-CORRELATED NMR SPECTROSCOPY (HSQC; HMQC) 271 9.4.4
THE GRADIENT-SELECTED (GS-)HMB 10.2.1 THE TWO-SPIN SYSTEM 298 10.2.2
ENHANCEMENT FACTORS 301 10.2.3 MULTI-SPIN SYSTEMS 302 10.2.4 FROM THE
ONE-DIMENSIONAL TO THE TWO-DIMENSIONAL EXPERIMENTS, NOESY AND ROESY 303
10.3 EXPERIMENTAL ASPECTS 305 10.4 APPLICATIONS 306 EXERCISES 311 10.5
BIBLIOGRAPHY FOR CHAPTER 10 311 11 DYNAMIC NMR SPECTROSCOPY (DNMR) .
313 11.1 INTRODUCTION 313 11.2 QUANTITATIVE CALCULATIONS 317 11.2.1
COMPLETE LINE-SHAPE ANALYSIS 317 LI.2.2 THE COALESCENCE TEMPERATURE 7C
AND THE CORRESPONDING RATE CONSTANT KC 319 11.2.3 ACTIVATION PARAMETERS
320 11.2.3.1 THE ARRHENIUS ACTIVATION ENERGY E\ 320 11.2.3.2 THE FREE
ENTHALPY OF ACTIVATION AG 321 11.2.3.3 ESTIMATING THE LIMITS OF ERROR
322 11.2.4 RATE CONSTANTS IN REACTIONS WITH INTERMEDIATE STAGES 323
11.2.5 INTERMOLECULAR EXCHANGE PROCESSES 324 11.3 APPLICATIONS 325
11.3.1 ROTATION ABOUT CC SINGLE BONDS 325 11.3.1.1 C(SP 3 )-C(SP 3 )
BONDS 326 11.3.1.2 C(SP 2 )-C(SP 3 ) BONDS 326 11.3.1. 13 NMR
SPECTROSCOPY IN BIOCHEMISTRY AND MEDICINE 355 13.1 INTRODUCTION 355 13.2
ELUCIDATING REACTION PATHWAYS IN BIOCHEMISTRY 355 13.2.1 SYNTHESES USING
SINGLY 13 C-LABELED PRECURSORS 356 13.2.1.1 LOW LEVELS OF 13 C
ENRICHMENT 356 13.2.1.2 HIGH LEVELS OF 13 C ENRICHMENT 357 13.2.2
SYNTHESES USING DOUBLY 13 C-LABELED PRECURSORS 358 13.3 BIOPOLYMERS 360
13.3.1 PEPTIDES AND PROTEINS 361 13.3.1.1 SEQUENCE ANALYSIS 362 13.3.1.2
THE THREE-DIMENSIONAL STRUCTURE OF PROTEINS. . 363 13.3.2
POLYNUCLEOTIDES 365 13.3.3 OLIGOSACCHARIDES AND POLYSACCHARIDES 367 13.4
SATURATION TRANSFER DIFFERENCE NMR SPECTROS- COPY (STD) 371 EXERCISES
372 13.5 BIBLIOGRAPHY FOR CHAPTER 13 372 14 IN VIVO NMR SPECTROSCOPY IN
BIOCHEMISTRY AND MEDICINE 375 14.1 INTRODUCTION 375 14.2 HIGH-RESOLUTION
IN VIVO NMR SPECTROSCOPY . . . 376 14.2.1 THE PROBLEM AND ITS SOLUTION
376 14.2.2 31 P NMR EXPERIMENTS 377 14.2.3 L N AND 13 C |
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| bvnumber | BV036668171 |
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| ctrlnum | (OCoLC)700438721 (DE-599)DNB100402410X |
| dewey-full | 543.66 |
| dewey-hundreds | 500 - Natural sciences and mathematics |
| dewey-ones | 543 - Analytical chemistry |
| dewey-raw | 543.66 |
| dewey-search | 543.66 |
| dewey-sort | 3543.66 |
| dewey-tens | 540 - Chemistry and allied sciences |
| discipline | Chemie / Pharmazie Biologie Chemie |
| edition | 5., completely rev. and enlarged. ed. |
| format | Book |
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| genre | (DE-588)4123623-3 Lehrbuch gnd-content |
| genre_facet | Lehrbuch |
| id | DE-604.BV036668171 |
| illustrated | Illustrated |
| indexdate | 2024-07-20T10:46:23Z |
| institution | BVB |
| isbn | 9783527327829 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-020587325 |
| oclc_num | 700438721 |
| open_access_boolean | |
| owner | DE-29T DE-20 DE-355 DE-BY-UBR DE-83 DE-11 DE-92 DE-634 DE-703 DE-188 DE-91G DE-BY-TUM DE-19 DE-BY-UBM |
| owner_facet | DE-29T DE-20 DE-355 DE-BY-UBR DE-83 DE-11 DE-92 DE-634 DE-703 DE-188 DE-91G DE-BY-TUM DE-19 DE-BY-UBM |
| physical | XXIV, 418 S. Ill., graph. Darst. |
| publishDate | 2011 |
| publishDateSearch | 2011 |
| publishDateSort | 2011 |
| publisher | Wiley-VCH |
| record_format | marc |
| spelling | Friebolin, Horst Verfasser (DE-588)106657968 aut Ein- und zweidimensionale NMR-Spektroskopie Basic one- and two-dimensional NMR spectroscopy Horst Friebolin 5., completely rev. and enlarged. ed. Weinheim Wiley-VCH 2011 XXIV, 418 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier nuclear magnetic resonance spectroscopy cabt Analytische Chemie (DE-588)4129906-1 gnd rswk-swf Methode (DE-588)4038971-6 gnd rswk-swf Zweidimensionale NMR-Spektroskopie (DE-588)4191219-6 gnd rswk-swf Dynamisches System (DE-588)4013396-5 gnd rswk-swf Polymere (DE-588)4046699-1 gnd rswk-swf Medizin (DE-588)4038243-6 gnd rswk-swf NMR-Spektroskopie (DE-588)4075421-2 gnd rswk-swf Biochemie (DE-588)4006777-4 gnd rswk-swf (DE-588)4123623-3 Lehrbuch gnd-content NMR-Spektroskopie (DE-588)4075421-2 s DE-604 Zweidimensionale NMR-Spektroskopie (DE-588)4191219-6 s 1\p DE-604 Analytische Chemie (DE-588)4129906-1 s 2\p DE-604 Medizin (DE-588)4038243-6 s 3\p DE-604 Biochemie (DE-588)4006777-4 s 4\p DE-604 Polymere (DE-588)4046699-1 s 5\p DE-604 Methode (DE-588)4038971-6 s 6\p DE-604 Dynamisches System (DE-588)4013396-5 s 7\p DE-604 text/html http://deposit.dnb.de/cgi-bin/dokserv?id=3498387&prov=M&dok_var=1&dok_ext=htm Inhaltstext DNB Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=020587325&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 4\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 5\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 6\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 7\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk |
| spellingShingle | Friebolin, Horst Basic one- and two-dimensional NMR spectroscopy nuclear magnetic resonance spectroscopy cabt Analytische Chemie (DE-588)4129906-1 gnd Methode (DE-588)4038971-6 gnd Zweidimensionale NMR-Spektroskopie (DE-588)4191219-6 gnd Dynamisches System (DE-588)4013396-5 gnd Polymere (DE-588)4046699-1 gnd Medizin (DE-588)4038243-6 gnd NMR-Spektroskopie (DE-588)4075421-2 gnd Biochemie (DE-588)4006777-4 gnd |
| subject_GND | (DE-588)4129906-1 (DE-588)4038971-6 (DE-588)4191219-6 (DE-588)4013396-5 (DE-588)4046699-1 (DE-588)4038243-6 (DE-588)4075421-2 (DE-588)4006777-4 (DE-588)4123623-3 |
| title | Basic one- and two-dimensional NMR spectroscopy |
| title_alt | Ein- und zweidimensionale NMR-Spektroskopie |
| title_auth | Basic one- and two-dimensional NMR spectroscopy |
| title_exact_search | Basic one- and two-dimensional NMR spectroscopy |
| title_full | Basic one- and two-dimensional NMR spectroscopy Horst Friebolin |
| title_fullStr | Basic one- and two-dimensional NMR spectroscopy Horst Friebolin |
| title_full_unstemmed | Basic one- and two-dimensional NMR spectroscopy Horst Friebolin |
| title_short | Basic one- and two-dimensional NMR spectroscopy |
| title_sort | basic one and two dimensional nmr spectroscopy |
| topic | nuclear magnetic resonance spectroscopy cabt Analytische Chemie (DE-588)4129906-1 gnd Methode (DE-588)4038971-6 gnd Zweidimensionale NMR-Spektroskopie (DE-588)4191219-6 gnd Dynamisches System (DE-588)4013396-5 gnd Polymere (DE-588)4046699-1 gnd Medizin (DE-588)4038243-6 gnd NMR-Spektroskopie (DE-588)4075421-2 gnd Biochemie (DE-588)4006777-4 gnd |
| topic_facet | nuclear magnetic resonance spectroscopy Analytische Chemie Methode Zweidimensionale NMR-Spektroskopie Dynamisches System Polymere Medizin NMR-Spektroskopie Biochemie Lehrbuch |
| url | http://deposit.dnb.de/cgi-bin/dokserv?id=3498387&prov=M&dok_var=1&dok_ext=htm http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=020587325&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT friebolinhorst einundzweidimensionalenmrspektroskopie AT friebolinhorst basiconeandtwodimensionalnmrspectroscopy |