简介:运用水热法合成了1个新的配合物[Ni(Phtpy)2](CH3COO)2(化合物1),(Phtpy=4′-苯基-2,2′∶6′,2″-三联吡啶),并通过X-射线单晶衍射方法确定了该化合物的晶体结构.结构分析表明化合物1属于三斜晶系,P-1空间群,晶胞参数a=0.90560(8)nm,b=1.10307(9)nm,c=2.02014(15)nm,α=94.3830(10)°,β=100.9830(10)°,γ=106.3120(10)°,V=1.8831(3)nm3,Z=2,R1=0.0872,wR2=0.1831.配合物中存在3种氢键和多种π-π相互作用,使其成为一个3D配合物.
简介:Thetitlecomplex,[La(baec)1/2(H2btec)1/2(H2O)]n(H4btec=1,2,4,5-benzenetetracarboxylicacid)(1)wassynthesizedbythehydrothermalreactionof1,2,4,5-benzenetetracarboxylicdianhydridewithLa(NO3)3·6H2OinH2O,andcrystallizesinthetriclinicsystem,spacegroupP-1withα=0.64403(3)nm,b=0.94500(4)nm,c=0.96380(5)nm,α=88.535(2)°,β=100.314(2)°,γ=76.6470(10)°,V=1.69968(10)nm^3,Z=2,andfinalR=0.0274,Rw=0.0735.In1,eachLa(Ⅲ)ioniscoordinatedbyeightoxygenatomsfromsixcarboxylategroupsandonecoordinatedwatermolecule.TwodifferentcoordinstionmodesofH4btecwerePresentinthestructure,oneofwhichcontainstwoprotonatedcarboxylategrougpstobalancethecharge.
简介:TostudytheintramolecularDiels-Aldercycloadditonof2H-chromen-2-oneasadiene,aseriesofchiralN-allyl-N-benzylamidesthatcontaina2H-chromen-2-onemoietyweredesignedforthesynthesisofbenzo[f]isoindol-l-onesviaanintramolecularDiels-Alderandasubsequentretro-Diels-AldercycloadditionwiththeexpulsionofCO2.Boththeyield(80%-89%)andabsolutestereocontrolofthetandemreactionwerehighwhenanelectron-withdrawinggroupwasattachedtothedienophile.Thedoublebondinthestyrenesubstructureremainedintheproductscouldbefurtherderivatizedbydihydroxylation.
简介:Three-dimensional(3D)flowerlikehierarchicalZn2GeO4andMn2+-dopedZn2GeO4microstructureshavebeenpreparedbyafacilehydrothermalapproach.X-Raydiffraction(XRD),fieldemissionscanningelectronmicro-scopy(FESEM),transmissionelectronmicroscopy(TEM)andphotoluminescence(PL)spectrometrywereemployedtocharacterizethesamples.SuchflowerlikehierarchicalZn2GeO4microstructureswithanaveragediameterof3―4μmwerefoundtobeconstructedbyabundantsinglecrystallinenanorodsofabout90nmindiameter.TheluminescentpropertiesofZn2GeO4:xMnphosphorswithdifferentcontentsofMn2+asanactivatorwereinvestigated.TheMn2+-dopedsamplesshowedgreenluminescencecorrespondingtothed-dtransitionofMn2+undertheirradiationofUVlight.Theredshift(from531nmto538nm)inλemwithincreasingMn2+contentwasobservedintheluminescentspectra,whichshouldbeattributedtoaweakcrystalfieldbecauseofthesubstitutionofZn2+byMn2+atadistortedtetrahedrallatticesite.
简介:通过5-甲基-7-甲氧基异黄酮与盐酸羟胺的缩合制得中间产物4-苯基-5-(2-羟基-4-甲氧基-6-甲基苯基)异恶唑,然后经过光异构化反应合成了4-甲氧基-6-甲基-7a-苯基苯并吡喃并[2,3-b]氮丙啶-7-酮,并采用IR,NMR,HRMS和单晶X-衍射分析对其结构进行了表征.单晶X-衍射分析结果表明:标题化合物属于单斜晶系,空间群P2(1)/n.在其晶体结构中,存在着氢键及芳香堆积作用,这些作用将标题化合物分子组装成了三维网络结构.
简介:AseriesofTiO2-XSiO2[Xdenotesthemolarfraction(%)ofsilicainthemixedoxides]withdifferentn(Ti)/n(Si)ratioswaspreparedwithammoniawaterasahydrolysiscatalyst.ThephotocatalystspreparedwerecharacterizedbyXRD,thermalanalysis,FTIR,UV-VisandSPS.ThecharacterizationresultsofFTIRandUV-VisspectrashowthatTiatomsweregraduallychangedfromoctahedralcoordinationtotetrahedralcoordinationwiththeadditionofsilica,whichisnotbeneficialforobtainingstrongBrnstedacidityandhigherphotocatalyticactivity.Thephotocatalyticactivityexperiments,whichwereconductedbyusingheptane(orSO2)asthemodelreactant,showedthatTiO2-SiO2containingasuitableamountofsilicacanexhibitmuchhigherphotocatalyticactivitythanpureTiO2.Theenhancedphotocatalyticactivitycanbeattributedtothreefollowingfactors:(1)smallercrystallinesize;(2)higherthermalstability;(3)thenewstrongBrnstedacidity.
简介:CarbonylationofAllylChlorideCatalyzedbyPdCl2(TPPTS)2inTwo-phaseMediumCarbonylationofAllylChlorideCatalyzedbyPdCl2(TPPTS)2in...
简介:ElectrolyticfixationofCO2wasinvestigatedbyelectrocarboxylationoforganichalides(RX),andfourestersⅠ,ⅡⅢ,Ⅳ)wereobtainedinmoderateyields.ElectrochemicalreductionesterificationsofRXinthepresenceofCO2werecarriedoutonnanocry'stallineTiO2-Ptelectrode.TheelectrochemicalbehaviorofRXinthepresenceofCO2wasinvestigatedbythetechniqueofcyclicvoltammetry,andtheprobablereactionmechanismw,asproposed.
简介:Emissionquenchingof[Ru(bpy)2(4,4’-dcbpy)](PF6)2(1)bybenzenamine,4-[2-[5-[4-[4-dimethylamino]phenyl]-4,5-di-hydro-1-phenyl-1H-pyrazol-3-yl]-ethenyl]-N,N-dimetyl(2)or1,5-diphenyl-3-(2-phenothiazine)-2-pyrazoline(3)wasobserved.Measurementsoftheemissiondecayof1beforeandafteradditionof2or3bysinglephotoncountingtechniquecon-finnedtheobservations.Theemissionquenchingof1by2or3wassubmittedtoStern-Volmerequation.Itwascalculatedthatthequenchingrateconstants(kq)are5.5×109(mol/L)-1s-1for2and4.0×109(mol/L)-1s-1for3,respectively.Theseresultsindicatedacharacterofdynamicquenchingprocess.Thesinglet-stateof2or3wasalsoquenchedby1.ThequenchingbehaviorsdidnotconformtotheStern-Volmerequationandinvolvedbothstaticanddynamicquenchingprocesses.Theapparentquenchingrateconstant(kapp)wascalculatedtobe3×109(mol/L)-1fortheinteractionofexcited2with1,and1.2×109(mol/L)-1forthatofexcited3wit
简介:采用水热法合成了一种新的超分子化合物{[2-(4-chlorophenyl)benzimidazoleH]2^2+·[SbCl5]^2-}n.通过元素分析、红外光谱、荧光光谱及X射线单晶衍射对其结构和性质进行了测定.结构分析表明;该晶体属于单斜晶系,P21/c空间群,晶胞参数为:a=0.5830(9)nm,b=1.6125(3)nm,c=1.6163(3)nm,β=94.181(2)°,Z=2,化学式为C26H20Cl7N4Sb,Mr=758.36,V=1.5155(4)nm^3,Dc=1.662g·cm^-3,μ=1.551mm^-1,F(000)=748,R1=0.0891,wR2=0.2568.Sb^3+与其周围6个氯离子配位,构成一个6配位的畸变八面体构型,配阴离子与2-(4-氯苯基)苯并咪唑阳离子以静电引力、氢键及π-π堆积作用形成三维网状超分子化合物.荧光测试显示该化合物具有较好的光致发光性能.
简介:HighactiveandstablegoldcatalystssupportedoncrystallineFe2O3andCeO2/Fe2O3werepreparedviathedeposition-precipitationmethod.ThecatalystwithaAuloadof1.0%calcinedat180°CshowedaCOconversionof100%at-8.9°C,whileAu/CeO2/Fe2O3convertedCOcompletelyat-16.1°C.Evenhavingbeencalcinedat500°C,Au/Fe2O3stillexhibitedsignificantcatalyticactivity,achievingfullconversionofCOat61.6°C.ThecatalystwithalowAuloadof0.5%couldconvertCOcompletelyatroomtemperatureandkepttheactivityunchangedforatleast150h.N2adsorption-desorptionmeasurementsshowthatthecrystallinesupportspossessedahighspecificsurfaceareaofabout200m2/g.CharacterizationsofX-raydiffractionandtransmissionelectronmicroscopyindicatethatgoldspecieswerehighlydispersedasnanoorsub-nanoparticlesonthesupports.Evenafterthecatalystwascalcinedat500°C,theAuparticlesremainedinanano-sizeofabout6―10nm.X-rayphotoelectronspectrarevealthatthesupportedAuexistedinmetallicstateAu0.ThemodificationofAu/Fe2O3byCeO2provedtobebeneficialtotheinhibitionofcrystallizationofFe2O3andthestabilizationofgoldparticlesindispersedstate,consequentlypromotingcatalyticactivity.
简介:利用水热法首次合成了具有两种配位环境Cd原子的新型杂多蓝化合物[NH3(CH2)2NH3]5[Cd(H2O)][CdMo12^vO30(HPO4)6(H2PO4)2]·5H2O.通过元素分析、ICP、TG和X射线单晶衍射确定了其组成,使用IR和EPR进行了结构表征.通过N2吸附脱附测定了比表面积和孔径,为催化研究提供了基础数据.结果表明:该晶体为三斜晶系,P-1,空间群;晶胞参数a=1.2002(2)nm,b=1.4651(3)nm,c=2.1192(4)nm,V=3.5642(12)nm^3,p=83.01(3)°,Z=2,F(000)=2932,R1=0.0300,wR2=0.0716.
简介:Yb3+complexeswithtwonitrilotriaceticacidmoleculeswerepreparedandtheircompositionsweredeterminedasK3[Yb(nta)2(H2O)]*5H2OandNa3[Yb(nta)2]*6H2Obyelementalanalyses.Theirstructureswerecharacterizedbysingle-crystalX-raydiffractionanalyses.IncomplexK3[Yb(nta)2(H2O)]*5H2O,theYbN2O7partformsanine-coordinatemonocappedsquareantiprismaticstructure.IncomplexNa3[Yb(nta)2]*6H2O,theYbN2O6partformsaneight-coordinatesquareantiprismaticstructure.Itcanbeseenthattheoutercations(K+andNa+)greatlyaffectthecoordinationnumberandcoordinatestructurefromtheseresults.