Nuclear Magnetic Resonance Volume 29

565 Pages·03.104 MB·565\565

A Specialist Periodical Report
Nuclear Magnetic Resonance
Volume 29
A Review of the Literature Published between
June 1998 and May 1999
Senior Reporter
G. A. Webb, Department of Chemistry, University of Surrey, Guildford, UK
Reporters
I. Barsukov, University of Leicester, UK
A.C. de Dios, Georgetown University, Washington, DC, USA
P.C. Driscoll, University College, London, UK
D. Esposito, University College, London, UK
H. Fukui, Kitami Institute of technology, Japan
E.F. Hounsell, Birbeck College, London, UK
C.J. Jameson, University of Illinois at Chicago, USA
K. .DPLH VND(cid:16)7UHOD, Polish Academy of Sciences, Warszaw, Poland
C.L. Khetrapal, University of Allahabad and Sanjay Gandhi Post Graduate
Institute of Medical Sciences, Lucknow, India
H. Kurosu, Nara Women’s University, Nara City, Japan
R. Ludwig, Universität Dortmund, Germany
G.A. Nagana Gowda, Indian Institute of Science, Bangalore, India
M Pfuhl, University College, London, UK
M.J.W. Prior, University of Nottingham, UK
K.V. Ramanathan, Indian Institute of Science, Bangalore, India
W. Schilf, Polish Academy of Sciences, Warszawa, Poland
M.E. Smith, University of Warwick, Coventry, UK
T. Watanabe, Tokyo University of Fisheries, Tokyo, Japan
J. Wójcik, Polish Academy of Sciences, Warszawa, Poland
M. Yamaguchi, Kao Corporation, Tochigi, Japan
T. Yamanobe, University of Gunma, Japan
Contents
Chapter1 NMRBooksandReviews 1
ByW.Schilf
1 Books 1
2 RegularReviewsSeries 2
3 EditedBooksandSymposia 5
4 ReviewsinPeriodicals 14
5 ReviewsandBooksinForeignLanguages 32
Chapter2 TheoreticalandPhysicalAspectsofNuclearShielding 41
ByC.J.JamesonandA.C.deDios
1 TheoreticalAspectsofNuclearShielding 41
1.1 GeneralTheory 41
1.2 AbInitioCalculations 54
2 PhysicalAspectsofNuclearShielding 58
2.1 AnisotropyoftheShieldingTensor 58
2.2 ShieldingSurfacesandRovibrationalAveraging 65
2.3 IsotopeShifts 70
2.4 IntermolecularE(cid:128)ectsonNuclearShielding 71
3 References 78
Chapter3 ApplicationsofNuclearShielding 85
ByM.Yamaguchi
1 Introduction 85
2 VariousChemicalandNuclearInfluencestoNuclearShieldings 85
2.1 ComputerAssistedStructuralAssignment 85
2.1.1 SpectrumSimulation,ComputerAssisted
AssignmentsandRelatedTechniques 85
2.1.2 NuclearShieldingCalculations 86
2.2 StereochemicalandNuclearShieldingNon-Equivalence 87
2.2.1ChiralityDeterminationbyMosher’sandRelated
Methods 87
2.2.2 OtherStereochemistryDetermination 88
2.3 IsotopeE(cid:128)ects 89
2.4 SubstituentE(cid:128)ects 89
2.4.1 ProtonSubstituentE(cid:128)ects 89
2.4.2 CarbonandHeteroatomSubstituentE(cid:128)ects 90
2.5IntramolecularHydrogenBondingE(cid:128)ectsandRelated
E(cid:128)ects 90
NuclearMagneticResonance,Volume29
#TheRoyalSocietyofChemistry,2000
vii
viii Contents
2.6 BondAnisotropy,RingCurrentE(cid:128)ectsandAromaticity 91
2.7 IntermolecularHydrogenBondingE(cid:128)ects,Inclusion
PhenomenaandRelatedE(cid:128)ects 91
2.7.1 ProtonandHeteronuclearShifts 92
2.7.2 Cyclodextrins(CDs) 92
2.7.3 OtherMolecularRecognition 93
2.8 ShiftReagent 93
2.9 MiscellaneousTopics 93
2.10 Reviews 94
3 ShieldingsofParticularNuclearSpecies 94
3.1 Group1(1H,2H,3H,6,7Li,23Na,87Rb,133Cs) 94
3.1.1 Hydrogen(1H) 94
3.1.2 Deuterium(2H) 95
3.1.3 Tritium(3H) 95
3.1.4 Lithium(6,7Li) 96
3.1.5 Sodium(23Na) 97
3.1.6 Rubidium(87Rb) 97
3.1.7 Caesium(133Cs) 98
3.2 Group2(9Be,25Mg,137Ba) 98
3.2.1 Beryllium(9Be) 98
3.2.2 Magnesium(25Mg) 98
3.2.3 Barium(137Ba) 98
3.3 Group3andLanthanoids(45Sc,89Y,139La,153Eu) 98
3.3.1 Scandium(45Sc) 98
3.3.2 Yttrium(89Y) 98
3.3.3 Lanthanum(139La) 99
3.3.4 Europium(153Eu) 99
3.4 Group4(47,47Ti) 99
3.5 Group5(51V,93Nb) 99
3.5.1 Vanadium(51V) 99
3.5.2 Niobium(93Nb) 101
3.6 Group6(95Mo,183W) 101
3.6.1 Molybdenum(95Mo) 101
3.6.2 Tungsten(183W) 101
3.7 Group7(55Mn,99Tc) 102
3.7.1 Manganese(55Mn) 102
3.7.2 Technetium(99Tc) 102
3.8 Group8(57Fe,99Ru) 102
3.8.1 Iron(57Fe) 102
3.8.2 Ruthenium(99Ru) 103
3.9 Group9(59Co,103Rh) 103
3.9.1 Cobalt(59Co) 103
3.9.2 Rhodium(103Rh) 103
3.10 Group10(195Pt) 104
3.10.1 Platinum(195Pt) 104
3.11 Group11(63Cu,107,109Ag) 106
3.11.1 Copper(63Cu) 106
3.11.2 Silver(107,109Ag) 106
3.12 Group12(67Zn,111,113Cd,199Hg) 106
3.12.1 Zinc(67Zn) 106
Contents ix
3.12.2 Cadmium(111,113Cd) 106
3.12.3 Mercury(199Hg) 107
3.13 Group13(11B,27Al,71Ga,203,205Tl) 108
3.13.1 Boron(11B) 108
3.13.2 Aluminium(27Al) 108
3.13.3 Gallium(71Ga) 109
3.13.4 Thallium(203,205Tl) 109
3.14 Group14(13C,29Si,73Ge,117,119Sn,207Pb) 109
3.14.1 Carbon(13C) 109
3.14.2 Silicon(29Si) 109
3.14.3 Germanium(73Ge) 112
3.14.4 Tin(117,119Sn) 112
3.14.5 Lead(207Pb) 115
3.15 Group15(14,15N,31P) 115
3.15.1 Nitrogen(14,15N) 115
3.15.2 Phosphorus(31P) 117
3.16 Group16(17O,33S,77Se,125Te) 117
3.16.1 Oxygen(17O) 117
3.16.2 Sulfur(33S) 118
3.16.3 Selenium(77Se) 118
3.16.4 Tellurium(125Te) 118
3.17 Group17(19F,35,37Cl) 119
3.17.1 Fluorine(19F) 119
3.17.2 Chlorine(35,37Cl) 119
3.18 Group18(3He,129Xe) 119
3.18.1 Helium(3He) 119
3.18.2 Xenon(129Xe) 120
4 References 120
Chapter4 TheoreticalAspectsofSpin-SpinCouplings 141
ByH.Fukui
1 Introduction 141
2 OriginoftheDiamagneticTerminFour-Component
RelatavisticCalculations 141
3 RovibrationalE(cid:128)ects 145
3.1 RovibrationallyAveragedSpin-SpinCouplingofthe
HydrogenFluorideMolecule 145
3.2 Spin-SpinCouplingSurfacesintheWaterMolecule,
OxoniumIon,andHydroxylIon 147
4 BasisSetDependenceofNuclearSpin-SpinCoupling
Constants 150
4.1 MulticonfigurationalSelf-ConsistentFieldCalculations 150
4.2 Second-OrderPolarizationPropagatorApproximation
Calculations 151
5 OtherAbInitioCalculations 154
6 DensityFunctionalTheoryCalculations 156
7 Semi-EmpiricalandOtherCalculations 159
8 References 161
x Contents
Chapter5 ApplicationsofSpin-SpinCouplings 165
ByK.Kamien´ska-TrelaandJacekWo´jcik
1 Introduction 165
2 Methods 166
3 One-BondCouplingstoHydrogen 171
4 One-BondCouplingsNotInvolvingHydrogen 174
5 Two-BondCouplingstoHydrogen 182
6 Two-BondCouplingsNotInvolvingHydrogen 183
7 Three-BondHydrogen-HydrogenCouplings 185
8 Three-BondCouplingsBetweenHydrogenandHeteronuclei 193
9 Three-BondCouplingsNotInvolvingHydrogen 198
10 CouplingsOverMoreThanThreeBonds 200
11 Non-TypicalCouplings 200
12 References 204
Chapter6 NuclearSpinRelaxationinLiquidsandGases 217
ByR.Ludwig
1 Introduction 217
2 General,PhysicalandExperimentalAspectsofNuclear
SpinRelaxation 219
2.1 GeneralAspects 219
2.2 ExperimentalAspects 221
2.3 RelaxationinCoupledSpinSystems 222
2.4 DipolarCouplingsandDistanceInformation 224
2.5 ExchangeSpectroscopy 226
2.6 RadiationDamping 228
2.7 QuadrupolarInteractions 229
2.8 IntermolecularDipolarInteractioninDiamagneticand
ParamagneticSolution 231
2.9 SlowMotionsinGlasses 233
2.10 ModelsforMolecularDynamics 235
3 SelectedApplicationsofNuclearSpinRelaxation 236
3.1 PureLiquids 236
3.2 Non-ElectrolyteSolutions 237
3.3 ElectrolyteSolutions 237
3.4 TransitionMetalComplexes 238
3.5 MoltenSalts 238
4 NuclearSpinRelaxationinGases 238
5 Self-Di(cid:128)usioninLiquids 240
5.1 ExperimentalandTheoreticalAspects 240
5.2 SelectedExamples 241
6 References 242
Chapter7 SolidStateNMR 251
ByM.E.Smith
1 Introduction 251
2 TechniqueDevelopment 252
2.1 Theoretical 252
2.2 Experimental 254
Contents xi
3 CarbonaceousMaterials 257
3.1 Coals,PitchesandOilShales 257
3.2 Fullerenes,DiamondsandOtherCarbons 258
4 OrganicMaterials 259
4.1 General 259
4.2 Organometallics 260
4.3 Bio-organic 262
4.4 LiquidCrystals,Membranes,Bilayers,CellWallsand
Woods 265
5 Organic-InorganicMaterials 267
5.1 General 267
5.2 SoilsandHumicSubstances 269
6 InorganicMaterials 269
6.1 General 269
6.2 SilicatesandAluminosilicates 272
6.3 MicroporousandMesoporousMaterials 274
6.3.1 Silicate-BasedSystems 274
6.3.2 OtherStructuralStudies 276
6.3.3 In-SituandSurfaceReactions 277
6.4 Glasses 279
6.5 Ceramics 280
7 Miscellaneous 281
7.1 General 281
7.2 DynamicsandIntercalates 282
8 References 283
Chapter8 MultiplePulseNMR 316
ByI.Barsukov
1 Introduction 316
2 VariationoftheRadiofrequencyPulse 317
2.1 SelectiveExcitation/InversionPulses 317
2.2 PulseFieldGradients 317
2.3 SolventSuppression 318
3 HomonuclearCorrelationSpectroscopy 318
4 NOE,ChemicalExchangeandRelaxation 319
4.1 NOEandChemicalExchange 319
4.2 RelaxationTimeMeasurements 321
4.3 TranslationalDi(cid:128)usionMeasurements 323
5 InverseProtonDetectedCorrelationSpectroscopy 324
5.1 General 324
5.2 IsotopeFilteredandEditedExperiments 324
5.3 ScalarCouplingConstantsMeasurements 325
5.3.1 QuantitativeJ-Correlation 325
5.3.2 E-COSY 326
5.3.3 Spin-StateSelectiveExperiments 327
5.3.4 Other 328
5.4 HeteronuclearDoubleResonanceExperiments 328
5.4.1 HSQC 329
5.4.2 HCCH 330
5.4.3 Other 331
xii Contents
5.5 HeteronuclearTripleResonanceExperiments 332
6 References 336
Chapter9 NMRofNucleicAcidsandProteins 340
ByP.C.Driscoll,D.EspositoandM.Pfuhl
1 Introduction 340
2 Proteins 341
2.1 LandmarkProteinStructures 341
2.2 Protein-LigandComplexes 343
2.3 Protein-LipidInteractions 344
3 NucleicAcids 346
3.1 RNAPsuedoknots 346
3.2 Double-IsotopeLabelledDNAMolecules 346
3.3 IonBindingtoNucleicAcids 348
3.4 NucleicAcidAdducts 349
3.5 NucleicAcidAptamers 350
4 TechnicalDevelopments 351
4.1 TransverseRelaxation-OptimisedSpectroscopy
(TROSY) 351
4.2 ScalarCouplingAcrossHydrogenBonds 354
4.3 LowViscositySolvents 356
4.4 StructuralRestraintsfromDatabases 357
4.5 J-Couplings 360
4.6 SoftwareDevelopments 361
4.7 SAR-by-NMR 363
4.8 ResonanceAssignmentsandPulseSequences 363
4.9 MacromolecularHydration 365
4.10 MethylProtonationinaDeuteratedBackground 366
4.11 SegmentallyLabelledProteins 368
4.12 StudiesofaProteinPhotointermediate 369
5 MeasurementsofResidualDipolarCouplings 370
5.1 Background 370
5.2 ResidualDipolarCouplingsinStructuralRefinement 371
5.3 LiquidCrystallineMediaforPartialAlignment 372
5.4 NewMethodsforMeasurementofResidualDipolar
Couplings 375
5.5 ImpactofResidualDipolarCouplingson
MacromolecularStructures 376
6 StudyofProteinDynamicsThroughHeteronuclear
RelaxationMeasurements 377
6.1 MethodologicalDevelopments 377
6.1.1 StudyofChemicalExchange 377
6.1.2 ImprovingtheAccuracyofRelaxation
ExperimentsandTheirInterpretation 379
6.1.3 RelaxationMeasurementsIncorporating15N
CSA/DipoleCrossCorrelation 381
6.1.4 MeasurementofSideChainDynamics 382
6.1.5 MechanisticInterpretationoftheDynamics
UnderlyingRelaxation 383
Contents xiii
6.2 Applications 384
6.2.1 Protein-NucleicAcidInteractions 384
6.2.2 Protein-ProteinInteractions 385
6.2.3 EnzymeFunction 388
6.2.4 Protein-MetalBinding 388
6.2.5 ProteinStructureandStability 389
6.2.6 ProteinFolding 391
6.2.7 Protein-LigandBindingE(cid:128)ects 392
6.2.8 RedoxProteins 394
6.2.9 DynamicsinMultidomainProteins 395
7 References 396
Chapter10 NMRofCarbohydrates,LipidsandMembranes 406
ByE.F.Hounsell
1 Introduction 406
2 PolysaccharidesandCyclodextrins 407
3 Carbohydrate-BasedNaturalProducts 409
4 MembraneStudies,GlycoproteinsandGangliosides 410
5 Proteoglycans 411
5.1Hyaluronan 412
5.2KeratanSulfate 412
5.3HeparinandHaparanSulfate 412
5.4ChondroitanSulfate 413
5.5OtherStudiesofUronicAcidsandSulfateEsters 413
6 BiomedicalApplications 413
7 References 413
Chapter11 SyntheticMacromolecules 419
ByH.KurosuandT.Yamanobe
1 Introduction 419
2 LiquidCrystals 419
3 PrimaryStructure 420
4 CharacterizationoftheSyntheticMacromolecules 420
5 DynamicsoftheSyntheticMacromolecules 436
6 GelsandCrosslinkedMacromolecules 437
7 PolymerBlendandDi(cid:128)usionoftheSyntheticMacromolecules 437
8 References 438
Chapter12 NuclearMagneticResonanceSpectroscopyofLivingSystems 453
ByM.J.W.Prior
1 GeneralApplicationsandNewMethodologies 453
1.1 Applications 453
1.2 SpectralEditing,SpectraAnalysis,Localisationand
Instrumentation 453
1.3 IntracellularIons,MetabolitesandpH 455
2 Cells 459
2.1 ReviewsandGeneralMethods 459
2.2 Bacteria 459
2.3 Blood 460
2.4 Mammalian 461
xiv Contents
2.5 Plant 462
2.6 Reproductive 463
2.7 Tumour 463
2.8 YeastandFungi 464
3 PlantsandAlgae 464
4 TissueStudies 466
4.1 BrainandSpinalCord 466
4.2 Eye 471
4.3 Heart 471
4.4 Kidney 481
4.5 Liver 481
4.6 ReproductiveSystem 483
4.7 SalivaryGlands 483
4.8 SkeletalMuscle 483
4.9 SmoothMuscle 484
4.10 Tumour 485
4.11 Skin 487
4.12 WholeAnimal 487
5 ClinicalStudies 488
5.1 Reviews 488
5.2 Brain 489
5.3 Heart 491
5.4 Liver 491
5.5 Muscle 492
5.6 Tumour 495
5.7 AdiposeTissue 495
6 References 496
Chapter13 NuclearMagneticResonanceImaging 509
ByT.Watanabe
1 Introduction 509
2 GeneralAspectsandReviews 510
3 Instruments 512
4 PulseSequencesandDataProcessing 513
5 SolidStateNMRImaging 516
6 OtherNuclei 517
7 Di(cid:128)usion,FlowandVelocityImaging 517
7.1 Di(cid:128)usionTensorImaging,Di(cid:128)usion-Weighted
ImagingandOne-DimensionalMapping 517
7.2 Flow,VelocityProfile,VelocityImaging,Rheometry 519
7.3 MassTransport,Absorption,Sedimentation,
Precipitation 520
8 Porosity,FluidAssistedImages 521
9 Polymers 522
10 Rock,Mineral,Clay,Coal 523
11 FoodandFoodProcessing 524
12 Plant 525
13 InVivo,ExVivoNMRImaging 527
13.1 1HNMRImaging(MT,Di(cid:128)usion,Functional,and
T *-WeightedImaging) 527
2
Contents xv
13.2 OtherNuclei-NMRImaging 528
13.3 ContrastEnhancedImagingviaParamagneticAgents 528
14 References 529
Chapter14 OrientedMolecules 534
ByC.L.Khetrapal,K.V.RamanathanandG.A.NaganaGowda
1 Introduction 534
2 Reviews,TheoryandGeneralStudies 534
3 EmergingAreasandNewTechniques 536
4 DynamicNMRStudies 540
5 Discotics,LyotropicsandChiralSystems 542
6 LiquidCrystalsinConfinedGeometriesandPolymeric
LiquidCrystals 544
7 MembranesandMoleculesOrientedbyThem 545
8 WeakOrderingandBiomolecularStudies 546
9 RelaxationStudies 551
10 MolecularOrder 552
11 StructureandConformation 556
12 References 557