Structure from Diffraction Methods: Inorganic Materials Series PDF
Preview Structure from Diffraction Methods: Inorganic Materials Series
Structure from Diffraction Methods InorganicMaterialsSeries SeriesEditors: ProfessorDuncanW.Bruce DepartmentofChemistry,UniversityofYork,UK ProfessorDermotO'Hare ChemistryResearchLaboratory,UniversityofOxford,UK ProfessorRichardI.Walton DepartmentofChemistry,UniversityofWarwick,UK SeriesTitles FunctionalOxides MolecularMaterials PorousMaterials Low-DimensionalSolids EnergyMaterials LocalStructuralCharacterisation MultiLength-ScaleCharacterisation StructurefromDiffractionMethods Structure from Diffraction Methods Edited by Duncan W. Bruce University of York, UK Dermot O'Hare University of Oxford, UK Richard I. Walton University of Warwick, UK Thiseditionfirstpublished2014 ©2014JohnWiley&Sons,Ltd Registeredoffice JohnWiley&SonsLtd,TheAtrium,SouthernGate,Chichester,WestSussex,PO198SQ,United Kingdom Fordetailsofourglobaleditorialoffices,forcustomerservicesandforinformationabouthowto applyforpermissiontoreusethecopyrightmaterialinthisbookpleaseseeourwebsiteat www.wiley.com. 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ISBN:9781119953227 Setin10.5/13ptSabonbyLaserwordsPrivateLimited,Chennai,India 12014 Contents InorganicMaterialsSeriesPreface xi Preface xiii ListofContributors xv 1 PowderDiffraction 1 KennethD.M.HarrisandP.AndrewWilliams 1.1 Introduction 1 1.2 TheSimilaritiesandDifferencesbetweenSingle-Crystal XRDandPowderXRD 2 1.3 QualitativeAspectsofPowderXRD:'Fingerprinting' ofCrystallinePhases 6 1.4 QuantitativeAspectsofPowderXRD:Some PreliminariesRelevanttoCrystalStructureDetermination 8 1.4.1 RelationshipbetweenaCrystalStructure anditsDiffractionPattern 8 1.4.2 ComparisonofExperimentalandCalculated PowderXRDPatterns 10 1.5 StructureDeterminationfromPowderXRDData 12 1.5.1 Overview 12 1.5.2 UnitCellDetermination(Indexing) 14 1.5.3 PreparingtheIntensityDataforStructure Solution:ProfileFitting 15 1.5.4 StructureSolution 16 1.5.5 StructureRefinement 21 1.6 SomeExperimentalConsiderationsinPowderXRD 22 1.6.1 SynchrotronversusLaboratoryPowder XRDData 22 1.6.2 PreferredOrientation 24 1.6.3 PhasePurityofthePowderSample 25 1.6.4 AnalysisofPeakWidthsinPowderXRDData 26 1.6.5 ApplicationsofPowderXRDforInSituStudies ofStructuralTransformationsandChemical Processes 28 vi CONTENTS 1.7 PowderNeutronDiffractionversusPowderXRD 30 1.8 ValidationofProceduresandResultsinStructure DeterminationfromPowderXRDData 33 1.8.1 Overview 33 1.8.2 ValidationbeforeDirect-SpaceStructure Solution 34 1.8.3 AspectsofValidationfollowingStructure Refinement 36 1.9 MoreDetailedConsiderationoftheApplication ofPowderXRDasa'Fingerprint'ofCrystallinePhases 40 1.10 ExamplesoftheApplicationofPowderXRDinChemical Contexts 44 1.10.1 Overview 44 1.10.2 StructureDeterminationofZeolitesandOther FrameworkMaterials 45 1.10.3 InSituPowderXRDStudiesofMaterials Synthesis 47 1.10.4 StructureDeterminationofNewMaterials ProducedbySolid-StateMechanochemistry 49 1.10.5 InSituPowderXRDStudiesofSolid-State MechanochemicalProcesses 52 1.10.6 InSituPowderXRDStudiesofaPolymorphic Transformation 54 1.10.7 InSituPowderXRDStudiesofaSolid-State Reaction 57 1.10.8 EstablishingDetailsofaHydrogen-Bonding ArrangementbyPowderNeutronDiffraction 57 1.10.9 StructureDeterminationofaMaterialProduced byRapidPrecipitationfromSolution 59 1.10.10 StructureDeterminationofIntermediates inaSolid-StateReaction 61 1.10.11 StructureDeterminationofaNovelAluminium Methylphosphonate 61 1.10.12 Structure Determination of Materials Prepared bySolid-StateDehydration/Desolvation Processes 62 1.10.13 StructureDeterminationoftheProductMaterial fromaSolid-StatePhotopolymerisation Reaction 65 1.10.14 ExploitingAnisotropicThermalExpansion inStructureDetermination 67 CONTENTS vii 1.10.15 RationalisationofaSolid-StateReaction 68 1.10.16 StructureDeterminationofOrganometallic Complexes 70 1.10.17 ExamplesofStructureDetermination ofSomePolymericMaterials 71 1.10.18 StructureDeterminationofPigmentMaterials 72 1.11 ConcludingRemarks 73 References 74 2 X-RayandNeutronSingle-CrystalDiffraction 83 WilliamClegg 2.1 Introduction 83 2.2 Solid-StateFundamentals 86 2.2.1 TranslationSymmetry 87 2.2.2 OtherSymmetry 91 2.2.3 AnIntroductiontoNon-IdealBehaviour 98 2.3 ScatteringandDiffraction 101 2.3.1 FundamentalsofRadiationandScattering 102 2.3.2 DiffractionofMonochromaticX-Rays 103 2.3.3 DiffractionofPolychromaticX-Rays 110 2.3.4 DiffractionofNeutrons 111 2.3.5 SomeCompetingandComplicatingEffects 114 2.4 ExperimentalMethods 119 2.4.1 RadiationSources 119 2.4.2 SingleCrystals 124 2.4.3 MeasuringtheDiffractionPattern 126 2.4.4 CorrectingforSystematicErrors 127 2.5 StructureSolution 128 2.5.1 DirectMethods 130 2.5.2 PattersonSynthesis 131 2.5.3 SymmetryArguments 132 2.5.4 ChargeFlipping 133 2.5.5 CompletingaPartialStructureModel 134 2.6 StructureRefinement 138 2.6.1 MinimisationandWeights 139 2.6.2 Parameters,ConstraintsandRestraints 139 2.6.3 RefinementResults 140 2.6.4 ComputerProgramsforStructureSolution andRefinement 141 viii CONTENTS 2.7 ProblemStructures,SpecialTopics,Validation andInterpretation 142 2.7.1 Disorder 142 2.7.2 Twinning 143 2.7.3 Pseudosymmetry,Superstructures andIncommensurateStructures 145 2.7.4 AbsoluteStructure 147 2.7.5 DistinguishingElementTypes,Oxidation StatesandSpinStates 148 2.7.6 ValenceEffects 149 2.7.7 DiffractionExperimentsunderNon-Ambient Conditions 150 2.7.8 IssuesofInterpretationandValidation 151 SoftwareAcknowledgements 153 References 153 3 PDFAnalysisofNanoparticles 155 ReinhardB.Neder 3.1 Introduction 155 3.2 PairDistributionFunction 160 3.3 DataCollectionStrategies 168 3.4 DataTreatment 170 3.4.1 CalculationofG(r)fromaStructuralModel 175 3.4.2 DataModelling 183 3.5 Examples 184 3.5.1 LocalDisorderversusLong-Range AverageOrder 185 3.5.2 ZnSeNanoparticle 189 3.5.3 DecoratedZnONanoparticle 194 3.6 ComplementaryTechniques 197 References 199 4 ElectronCrystallography 201 LuHan,KeiichiMiyasakaandOsamuTerasaki 4.1 Introduction 201 4.2 CrystalDescription 203 4.2.1 FourierTransformationandRelated Functions 203 4.2.2 Lattices 204
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