NMR of paramagnetic molecules: applications to metallobiomolecules and models
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| Main Authors: | , , , |
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| Format: | Book |
| Language: | English |
| Published: |
Amsterdam
Elsevier
[2017]
|
| Edition: | Second edition |
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Physical Description: | xii, 495 Seiten Illustrationen, Diagramme |
| ISBN: | 9780444634368 |
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MARC
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Record in the Search Index
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| adam_text | Contents
Preface ’ xi
CHAPTER 1 Introduction 1
1 1 Magnetic Moments and Magnetic Fields 1
1 2 About the Spin Moments 3
1 3 Something More About the Nuclear Spin 6
14A Lot More About the Electron Spin 8
1 5 About the Energies 12
1 6 Magnetization and Magnetic Susceptibility 12
1 7 The Nuclear Magnetic Resonance Experiment 17
171 The Pulse Experiment and Definition of Tx and T2 17
172 The Chemical Shift 18
173 Something More About Relaxation Rates 21
General References 23
References 24
CHAPTER 2 The Hyperfine Shift 25
2 1 Nuclear Hyperfine Shift and Relaxation 25
211 The Spin Density 26
2 2 The Magnetic Nucleus-unpaired Electron Interaction: The Hyperfine Shift 27
221 The Fermi Contact Coupling 27
2 3 Shift and Spin Patterns for Protons and Deuterons in Solution 43
231 Metal Ion-Water Interactions 45
2 4 Proton Hyperfine Coupling and Conformation 47
2 5 The Origin of the Shifts in Heteronuclei 49
2 6 When is Metal-Centered Pseudocontact Shift Expected? 55
2 7 Attempts to Separate Contact and Pseudocontact Shifts 56
2 8 Prediction of Hyperfine Shifts 57
References 58
CHAPTER 3 The Effect of Partial Orientation: Residual Dipolar Couplings 6i
3 1 Partial Orientation Effects on Nucleus-Nucleus Dipolar Coupling 61
3 2 The Magnetic Field Induced Order 64
3 3 Paramagnetic Metal Ions and Residual Dipolar Couplings 66
3 4 Residual Dipolar Couplings in the Presence of Diamagnetic
and Paramagnetic Anisotropy 71
3 5 Partial Orientation Effects on the Dipolar and Contact Shifts 73
V
VI
Contents
351 Partial Orientation Effects on the Pseudocontact Shifts 73
352 Partial Orientation Effects on the Contact Shifts 75
General References 75
References 75
CHAPTER 4 Relaxation 77
4 1 Introduction 77
4 2 The Correlation Time 79
4 3 Electron Relaxation 82
431 The Main Mechanisms for Electron Relaxation 85
4 4 Nuclear Relaxation due to Dipolar Coupling with Unpaired Electrons 89
441 Generalized Dipolar Coupling 93
4 5 Nuclear Relaxation due to Contact Coupling with Unpaired Electrons 94
4 6 Curie Nuclear Spin Relaxation 95
4 7 Further Electronic Effects on Nuclear Relaxation 98
471 The Effect of g Anisotropy and of the Splitting of the S Manifold
at Zero Magnetic Field 98
472 Field Dependence of Electron Relaxation 101
48A Comparison of Dipolar, Contact, and Curie Nuclear Spin Relaxation 103
4 9 Cross Correlation Effects 105
4 10 Nuclear Parameters and Relaxation 107
4 11 The Effect of Temperature on the Electron-Nucleus Spin Interaction 108
4 12 Stable Free Radicals 109
4 13 Redfield Limit and Beyond 110
4 14 The Nuclear Overhauser Effect Ill
4 14 1 Steady State NOE 112
4 14 2 Steady State NOE in Real Life 114
4 14 3 Selective and Nonselective Tx 115
4 14 4 Steady State NOE in Paramagnetic Compounds 117
4 15 Overhauser DNP 118
References 123
CHAPTER 5 High Resolution Solid-State NMR in Paramagnetic
Molecules 127
5 1 Nuclear Interactions in Solid-State NMR: Static and MAS 127
511 The Spatial Dependence of Nuclear Interactions 127
512 Magic Angle Spinning (MAS) 128
513 Homonuclear Coupling and Its Implications
for Heteronuclear Decoupling 133
514 Recoupling 134
5 2 NMR Spectra of Paramagnetic Complexes in the Solid State 135
521 The Effect of Paramagnetic Centers 135
522 Proton-Enhanced Spectroscopy 137
Contents vii
523 Measurement of Paramagnetic Interactions
and Their Anisotropy 140
524 Description of Crystal Lattices (Complexes and Proteins) 141
5 3 Dynamic Nuclear Polarization in the Solid State 142
531 Solid Effect 143
532 Cross Effect in Static and Rotating Solids, Comparison
of DNP Efficiencies and Radical Design 145
References 149
CHAPTER 6 Chemical Exchange, Chemical Equilibria,
and Dynamics m
6 1 Introduction 151
62A Pictorial View of Chemical Exchange 152
6 3 NMR Parameters in the Presence of Exchange 154
631 Exact Solutions for Two-Site Exchange 154
632 Exchange of Excess Metal Ligands 156
633 Temperature and Exchange 159
634 Saturation Transfer 160
6 4 Equilibrium Constants 162
641 NMR of Metal Ligands 162
642 NMR of Water Protons (The Enhancement Factor) 163
6 5 tm as Correlation Time 165
6 6 Beyond the Concept of Binding Site: Outer Sphere Relaxation 165
6 7 Solvent Relaxivity and Its Information Content 168
6 8 Bulk Susceptibility Shift 170
References 172
CHAPTER 7 Transition Metal Ions: Shift and Relaxation 175
7 1 An Overview of the Electronic Properties of Transition Metal Ions 175
711 Introductory Remarks on the Electronic Structure of Metal Ions 175
712 Electron Relaxation for the Different Metal Ions 177
713 Magnetic Susceptibility Anisotropy for the Different Metal Ions 180
72A Quick Summary of First Row Transition Metal Ions 180
721 Titanium 181
722 Vanadium 181
723 Chromium 181
724 Manganese 181
725 Iron 181
726 Cobalt 182
727 Nickel 182
728 Copper 182
7 3 Properties of Paramagnetic Ions Sorted by Electron Configuration 182
731 dVd9 (Cu2+, Ti3+, V02+) 182
732 d2/d8 (Ni2+, V3+) 200
Contents
viii
733 d3 (Cr3+) 203
734 d4 (Mn3+, Iron(IV)) 206
735 d5 (Fe3+,Mn2+) 208
736 d6 (Fe2+) 235
737 d7 (Co2+, Ni3+) 240
References 249
CHAPTER 8 Lanthanoids and Actinoids: Shift and Relaxation 255
8 1 Electronic Properties 255
8 2 The Pseudocontact Contribution to the Hyperfine Shifts 256
8 3 The Contact Contribution to the Hyperfine Shifts 258
8 4 Analysis of the Hyperfine Shifts 258
841 Separation of Pseudocontact and Contact Contributions 258
842 Limitations of Bleaney’s Theory 260
8 5 Nuclear Spin Relaxation 260
8 6 Gadolinium 261
8 7 Europium(II) 264
8 8 Other Lanthanoids 265
References 274
CHAPTER 9 Paramagnetic Restraints for Structure and Dynamics
of Biomolecules 277
9 1 Why Using Paramagnetic Restraints for Structural Biology Studies? 277
9 2 Nuclear Relaxation Parameters and Structural Information 278
921 Molecules Containing Paramagnetic Centers 278
922 Solvent Paramagnetic Molecules 284
9 3 Hyperfine Shifts and Structural Information 285
9 4 Paramagnetic Residual Dipolar Couplings and Structural Information 289
9 5 Protocols for Structural Determination Through Paramagnetic Data 290
951 Ab initio Protein Structure Determination 291
952 Refinement of Available Protein Models 294
953 Assembly of Rigid Substructures 296
9 6 Average Data in the Presence of Conformational Variability 298
9 7 Tagged Proteins 303
9 8 Structural Information from Pseudocontact Shifts in the Solid State 305
Web Sites of Main Programs for the Use of Paramagnetic Restraints
for Structure and Dynamics 308
References 308
CHAPTER 10 Relaxometry and Contrast Agents for MRI 313
10 1 Introduction 313
10 2 Relaxivity and Relaxation Profiles 314
Contents
ix
10 3 The Ideal Contrast Agent 317
10 4 NMRD-derived Parameters 323
10 4 1 Coordinated Protons and Their Distance 323
10 4 2 Reorientation, Electron Relaxation, and Residence Times 324
10 4 3 Best Fit Programs 325
10 5 NMRD Profiles of Contrast Agents 327
10 5 1 Small Molecule Contrast Agents 327
10 5 2 Functionalized Contrast Agents 330
10 5 3 High-field Contrast Agents 332
10 6 Nanosystems 334
10 7 Toward Molecular Imaging 338
10 8 Superparamagnetism 340
10 9 Chemical Exchange Saturation Transfer (CEST) 341
General References 343
References 343
CHAPTER 11 Magnetic Coupled Systems 347
11 1 The Induced Magnetic Moment Per Metal Ion in Polymetallic Systems,
the Hyperfine Contact Shift, and the Nuclear Relaxation Rates 347
11 2 Electron Relaxation and Magnetic Coupling 352
11 2 1 Homodimers 353
11 2 2 Heterodimers 354
11 2 3 Polymetallic Systems 355
11 3 NMR of Dimetallic Systems 356
11 3 1 Systems Containing Equal Metal Ions, 171 JcT 356
11 3 2 Systems Containing Equal Metal Ions, 171 « kT 356
11 3 3 Systems Containing Different Metal Ions, 171 kT 360
11 3 4 Systems Containing Different Metal Ions, 171 = kT 364
11 4 Beyond the Redfield Limit: 1711h t1 366
11 5 Polymetallic Systems 369
11 5 1 The [(RS)3Fe3S4]2_ Case 372
11 5 2 The [(RS)nCo4]3_ Case 372
11 5 3 The [(RS)4Fe4S4]x~ (X = 1,2,3) Case 375
11 5 4 The [(RS)3LFe3NiS4]3” Case 379
References 379
CHAPTER 12 Hints on Experimental Techniques 383
12 1 How to Record ID NMR Spectra of Paramagnetic Molecules 383
12 1 1 Presaturation Sequences 386
12 1 2 Selective Nonexcitation 389
12 1 3 Selective Suppression of Signals with Long Tx 390
12 1 4 Choice of Magnetic Field 392
12 1 5 Experimental Accessibility of Nuclear Relaxation Parameters 395
X
Contents
12 2 Measurements of Nuclear Overhauser Effect (NOE) 399
12 3 ND Spectroscopy 407
12 3 1 Solution NMR—EXSY and NOESY 409
12 3 2 Solution NMR—COSY 425
12 3 3 Solution NMR—TOCSY 432
12 3 4 Solution NMR—Heteronuclear Correlation Experiments 435
12 3 5 Solution NMR—3D Experiments 439
12 3 6 Solid-State NMR—Homonuclear Experiments 443
12 3 7 Solid-State NMR—Heteronuclear Correlation Experiments
and Proton Detection 444
12 3 8 Solid-State NMR—Lineshape Analysis Methods 445
12 4 Collecting Paramagnetic Restraints in Biomolecules 447
12 5 Nuclear Magnetic Relaxation Dispersion (NMRD) 448
12 5 1 Changing the Magnetic Field 448
12 5 2 Field-cycling Relaxometry 449
References 452
APPENDIX I NMR Properties of Nuclei 457
APPENDIX II Dipolar Coupling Between Two Spins 461
APPENDIX III Derivation of the Equations for Contact Shift
and Relaxation in a Simple Case 463
APPENDIX IV Derivation of the Pseudocontact Shift Equations
in Different Forms 467
APPENDIX V Relaxation by Dipolar Interaction Between Two Spins 471
APPENDIX VI Calculation of (S2): Curie’s Law 477
APPENDIX VII Derivation of the Equations Related to NOE 479
APPENDIX VIII Magnetically Coupled Dimers in the High-temperature Limit 483
APPENDIX IX Reference Tables 485
Index
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| any_adam_object | 1 |
| author | Bertini, Ivano Luchinat, Claudio Parigi, Giacomo Ravera, Enrico |
| author_GND | (DE-588)184119146 |
| author_facet | Bertini, Ivano Luchinat, Claudio Parigi, Giacomo Ravera, Enrico |
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| discipline | Chemie / Pharmazie |
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| id | DE-604.BV043685981 |
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| indexdate | 2024-07-10T07:32:29Z |
| institution | BVB |
| isbn | 9780444634368 |
| language | English |
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| spelling | Bertini, Ivano Verfasser aut NMR of paramagnetic molecules applications to metallobiomolecules and models Ivano Bertini ; Claudio Luchinat ; Giacomo Parigi ; Enrico Ravera Second edition Amsterdam Elsevier [2017] © 2017 xii, 495 Seiten Illustrationen, Diagramme txt rdacontent n rdamedia nc rdacarrier Paramagnetismus (DE-588)4173291-1 gnd rswk-swf Biomolekül (DE-588)4135124-1 gnd rswk-swf Magnetische Kernresonanz (DE-588)4037005-7 gnd rswk-swf Paramagnetismus (DE-588)4173291-1 s Magnetische Kernresonanz (DE-588)4037005-7 s DE-604 Biomolekül (DE-588)4135124-1 s Luchinat, Claudio Verfasser aut Parigi, Giacomo Verfasser (DE-588)184119146 aut Ravera, Enrico Verfasser aut HEBIS Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=029098760&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Bertini, Ivano Luchinat, Claudio Parigi, Giacomo Ravera, Enrico NMR of paramagnetic molecules applications to metallobiomolecules and models Paramagnetismus (DE-588)4173291-1 gnd Biomolekül (DE-588)4135124-1 gnd Magnetische Kernresonanz (DE-588)4037005-7 gnd |
| subject_GND | (DE-588)4173291-1 (DE-588)4135124-1 (DE-588)4037005-7 |
| title | NMR of paramagnetic molecules applications to metallobiomolecules and models |
| title_auth | NMR of paramagnetic molecules applications to metallobiomolecules and models |
| title_exact_search | NMR of paramagnetic molecules applications to metallobiomolecules and models |
| title_full | NMR of paramagnetic molecules applications to metallobiomolecules and models Ivano Bertini ; Claudio Luchinat ; Giacomo Parigi ; Enrico Ravera |
| title_fullStr | NMR of paramagnetic molecules applications to metallobiomolecules and models Ivano Bertini ; Claudio Luchinat ; Giacomo Parigi ; Enrico Ravera |
| title_full_unstemmed | NMR of paramagnetic molecules applications to metallobiomolecules and models Ivano Bertini ; Claudio Luchinat ; Giacomo Parigi ; Enrico Ravera |
| title_short | NMR of paramagnetic molecules |
| title_sort | nmr of paramagnetic molecules applications to metallobiomolecules and models |
| title_sub | applications to metallobiomolecules and models |
| topic | Paramagnetismus (DE-588)4173291-1 gnd Biomolekül (DE-588)4135124-1 gnd Magnetische Kernresonanz (DE-588)4037005-7 gnd |
| topic_facet | Paramagnetismus Biomolekül Magnetische Kernresonanz |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=029098760&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
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