单晶衍射仪Apex II使用系列教程-1PPT文档格式.pptx

单晶衍射仪Apex II使用系列教程-1PPT文档格式.pptx

《单晶衍射仪Apex II使用系列教程-1PPT文档格式.pptx》由会员分享，可在线阅读，更多相关《单晶衍射仪Apex II使用系列教程-1PPT文档格式.pptx（95页珍藏版）》请在冰豆网上搜索。

ThomasC.Furnas;

SiemPootWilliamR.BusingHenriA.LevyJohnS.RollettHereisthefrontcoverofTomFurnasexcellenttreatiseonsingle-crystaldiffractometrytheSCOIM,aswecalledititcanstillbefoundifyouhavethetimeandinterest!

.andherestheTitlePitawgaes:

aproductoftheGeneralElectricX-rayDepartment!

CONTENTSThefollowinglinksprovidenavigationonceyouhavestartedtousethetutorial,butpleasebeginbyselectingUnit1below（later,youcanreturnhereorleavethetutorialbypushingtheESCkeyoneormoretimes）:

（blackinktopicsareunderdevelopment）:

1.Chapter1.ppt2.Apex2QuickTricks,SidebarsandHOWTOs3.TwinnedCrystals;

StrangeandNearlyAwfulSamples4.ABriefPictorialHistoryofSingle-CrystalDiffractometry5.OrientationMatrixOperations;

PhaseTransitions&

Topotaxy6.Credits:

ExactwebaddressofalllinksincludedinVersion1.xxChapter1Apex2:

AtutorialusingtheYlidStandardCrystalBeforeplacingthistutorialontheweb,Iletafewofmyfriendsseeanearlierversion,andaskedthattheyprovidebothcommentsandcorrections.Unlikepreviouspasses,whereIobtainedcommentsonmySpaceGroupandHighSchoolCrystallographytutorials,Ilearnedquicklythattherewerecommentsthatcorrectederrors,andothersthatrepresented“localapproaches”.ThelatterrangedfromsomeverycoolthingswhichIincorporated,topreferencesthatIdidnotwishtoinclude,rathertakingadifferentapproachinmyownlaboratory.Ourtechniquesusuallyresultinvaluesof0.009-0.030fortheconventionalR-factor.Sooo.whenyougothroughthisandlaterversions,youllfindourapproachtodatacollectionandanalysis.Ifyouareanexperienceduser,nodoubtyoullseethingsthatyoudodifferentlyanddonotwishtochange:

thatsfine.Youmaychangetherawpowerpointtosuityourpreferences,butIask,then,thatyoudonotdistributeitwithoutnotingthatyouhavealteredslidesoncertainpages,asnoted.Addaslideatthebeginningtoindicate“whosayswhat”!

AllthatistheninconcertwiththeCreativeCommonsAttribution3.0UnportedLicense.Important:

HowToUseandDistributeThisTutorialBeforeyourinstrumentleftthefactory,thefolkstherecollecteddatausingtheBrukerStandardCrystal（anylidfirstchosenintheearlydaysofdiffractometrybyArildChristensenofSyntexAnalyticalInstruments）.YoucanreadmoreaboutthisinanicestudycarriedoutbyIliaGuzeioftheUniversityofWisconsin.1Whenyourinstrumentwasinstalled,thedatasetwasrecollectedunderthesameconditionsforcomparisonbeforetheinstallationwascertified.TheYliddatasetcanusuallybefoundunderthename“cust”inyourstructuredirectory.Thisisasmallbutusefuldataset,withfourstandard“runs”（moreaboutthatlater）,whichiscollectedinarelativelyshorttime.InthisChapterwewillcollectdataonanYlidstandardcrystal,butwellcarryouta24-hourdatacollection.Itwillbeofsomeinteresttobrieflycomparethetwodatacollections.ThepresentChapteroutlinesthesetupandexecutionofa“long”Ylidrun,and,attheend,makessomeobservationsaboutthedifferencesinstatisticalqualityofthe“cust”andthe“long”datasets.Therewillbe“how-tos”,aswellas“whys”hopefullyyouwillfindthemixofpedagogyandinstructionhelpful.Noteverythingwillbeexplainedimmediately,sinceweneedtolearnsomethingoftheoperationsfirst,butaswegothroughlaterexamples,wewillconsidersomeofthedeeperissuesindiffractometryandX-raycrystallography.1Guzei,I.A.;

Bikzhanova,G.A.;

Spencer,L.C.;

Timofeeva,T.V.;

Kinnibrugh,T.l.;

Campana,C.F.Cryst.GrowthDes.2008,8,24112418.“TheYlid”:

C11H10O2STheMan:

ArildChristensenTheMolecule:

ArildsYlidThecrystal,groundtoasphericalshapeThepaper（DOIlink）WellnowassumethatwevemountedourYlidStandardCrystalontheinstrument,andcentereditintheX-raybeam.WepunchtheApex2logoonourcomputernearthediffractometer,andwereaway:

First,weselect“New”onthe“Sample”tab.Thenthisscreenpopsup.Wepickasensiblename（alacompound,notebooknumber,userinitials&

cbolamhp,obulanhd,bla