FullProf-详细使用教程

Durban,August24,2003ECM-21SoftwareWorkshopRietveldrefinementofcomplexinorganicmaterialsusingFullProf(Extendedversionintutorialform)JuanRodríguez-CarvajalLaboratoireLéonBrillouin(CEA-CNRS),CEA/SaclayFRANCEDurban,August24,2003ECM-21SoftwareWorkshopAprogramforanalysisofdiffractionpatterns:FullProf•Aprogramfor:SimulationofpowderdiffractionpatternsPatterndecompositionÖintegratedintensitiesStructurerefinementPowderandsinglecrystaldata•Crystalandmagneticstructures•Multipledatasets:simultaneoustreatmentofseveralpowderdiffractionpatterns(CWX-rays&neutrons,EnergydispersiveX-rays,TOFneutrondiffraction)•Combinedtreatmentofsinglecrystalandpowderdata•CrystalandmagneticStructuredeterminationcapabilities:simulatedannealingonintegratedintensitydataDurban,August24,2003ECM-21SoftwareWorkshopHowworksFullProfFullProfOutputfiles,Plotdiffr.patternsMinimalinput:Inputcontrolfile(extension‘.pcr’):PCR-fileModel,crystallographic/magneticinformationPCRfileDATfile(s)Eventually,experimentaldataDurban,August24,2003ECM-21SoftwareWorkshopThePCRfile:steeplearningcurveDATfile(s)Formatdependingontheinstrument,usuallysimpleÄManyvariablesandoptionsÄComplextohandlePCRfileÄHint:copyanexisting(working)PCR-fileandmodifyitfortheusercase,or...ÄUSEthenewGUI:EdPCRDurban,August24,2003ECM-21SoftwareWorkshopLastminutechangesinFullProfDocumentedin“fp2k.inf”--------------------------------------------------------------------------Inthisfilenewfeatures,aswellasdiscoveredbugs,ofFullProf.2kareperiodicallydocumented.FordetailsconsultthemanualofFullProf.From10May2003,commentsontheprogramsconstitutingtheFullProfsuitearealsoprovided.JuanRodriguez-Carvajal(LaboratoireLeonBrillouin,Saclay)-----------------------------------------------------------------------------------------28July2003----------------AnupdatedversionofFullProf.2kisnowavailable..........-Somechangeshavebeenintroducedfortreatingthebackground:(1)Thepolynomialbackgroundof12coefficients,forconstantwavelengthcase,hasbeenchangedsothatthelastthreecoefficientscorrespondtoinversepowersof2theta........(2)Nowthereisthepossibilitytoincludeseveralpreviouslycalculatedprofilesascontributing,throughalinearcombination,tothebackgroundofapowderdiffractionpattern.Theindividualprofilesarereadininputfilesnamedfiledat_n.bac.Wherefiledatisthecodeofthedatafilecorrespondingtoadiffractionpatternandtheindexnisthenumberofthecontributingprofile.Theadditionalcontributiontothebackgroundiscalculatedas:Durban,August24,2003ECM-21SoftwareWorkshopLastminutechangesinFullProfDocumentedin“fp2k.inf”-ReorganizationoftheTOFpeakshapesandderivatives.Therefinementoftheinstrumentalparametersisnowmuchmorestable......ThenewpeakshapeINSTR=13(thankstoLaurentChapon!)consistingintheconvolutionofapseudo-VoigtfunctionwiththeIkeda-Carpenterfunctionisnowworking.TheTOFpeakshapesusedinFullProfandthemeaningofeachrefinableparameterisnowdocumentedinthenote:TOF_FullProf.PDFDurban,August24,2003ECM-21SoftwareWorkshopSomerecentfeaturesinFullProfÄNewfacilitiesconcerningsymmetryÄAutomaticmodeforhandlingrefinementcodesandsymmetryconstraintsÄTheuseofdistancesandanglesrestraintsÄChangesintheformatofthefilecontainingtheInstrumentalResolutionFunctionÄSpecialformfactorsÄSimulatedAnnealingÄThetreatmentofmicro-structuraleffectsDurban,August24,2003ECM-21SoftwareWorkshopNewfacilitiesconcerningsymmetryinFullProf⇒ThesymmetryusedwithinFullProfistotallybasedintheCrystallographicFortran95ModulesLibrary(CrysFML)(Tuesday26⇒FA3-MS5,MeetingRoom11B)⇒Thesemodulesprovidebettercrystallographicinformationtotheuseroftheprogram.Inparticularautomaticcalculationofthemultiplicityofeachsiteisnowperformedafterreadingtheatomsaswellasthecalculationoftheappropriatecoefficientsforautomaticquantitativeanalysisofmixtureofphases.⇒Newoutputfileswithfullinformationofcrystallographicsymmetryareproduced(extension:sym)Durban,August24,2003ECM-21SoftwareWorkshopSimulatedAnnealinginFullProfDurban,August24,2003ECM-21SoftwareWorkshopThestructureofacidstrontiumoxalatewasdeterminedfromX-raypowderdiffractionG.Vanhoylandetal.JSSC157,283(2001)Therawchemicalcompositionshouldbe:SrC3O7H3Wherearethehydrogenatoms?Neutronpowderdiffractiongivesyoutheanswer…Durban,August24,2003ECM-21SoftwareWorkshopThestructureofacidstrontiumoxalatewasdeterminedfromX-raypowderdiffractionG.Vanhoylandetal.JSSC157,283(2001)Wherearethehydrogenatoms?IntheoriginalpaperhydrogenatomsweredeterminedusingFouriersynthesis.HereweusethispublishedexampletoillustratehowtousetheSimulatedAnnealingoptionexistinginFullProfDurban,August24,2003ECM-21SoftwareWorkshopComparisonofthe“x-raystructure”withtheobservedneutronpowderdiffractionpatternofacidStrontiumoxalate.Thermalparametersarewrong…needrefinementofsomeBiso!Durban,August24,2003ECM-21SoftwareWorkshopComparisonofthe“x-raystructure”withtheobservedneutronpowderdiffractionpatternofacidStrontiumoxalate.AfterrefinementofbackgroundandB(Sr),B(C)andB(O)Durban,August24,2003ECM-21SoftwareWorkshopPortionofPCR(AcidSr-oxalate)filetoperformaLeBailfitwithoutputofanintegratedintensityfilesuitableforSimulatedAnnealing.......!--