简介:采用2步水热法合成了LaPO4∶Eu3+-Fe3O4复合材料.在LaPO4∶Eu3+-Fe3O4复合材料中,LaPO4∶Eu3+为单斜晶相,呈纳米棒状,纳米棒的直径和长度分别为20-100nm和0.2-1μm;Fe3O4为正交晶相、呈20-30nm的颗粒状,Fe3O4粒子紧紧附着在LaPO4∶Eu3+纳米棒的表面;样品的磁性和发光性质研究表明所合成的LaPO4∶Eu3+—Fe3O4复合材料既具有发光性质又具有磁性.
简介:Thetetranuclearalkyltin(Ⅳ)compounds{[R2Sn(C9H8N3O3)O]SnR3}2[R=n-Bu(1),4-CNC6H4CH2(2),C6H5CH2(3),4-ClC6H4CH2(4)]werepreparedbythereactionofSchiffbaseligandpyruvicacidisonicotinylhydrazonewith(R3Sn)2Ointhecorrespondingmolarratioof1:1.Allcompoundshavebeencharacterizedbyelementalanalysis,IRand^1HNMRspectra.Thecrystalstructureofcompound1wasdeterminedbyX-raysinglecrystaldiffractionalanalysis.Thiscompoundexhibitsadimericstructurecontainingdistannoxaneunitswithtwotypesofthetinatoms.Forthefirsttinatom,itappearstobeseven-coordinatedwithadistortedpentagonalbipyramidgeometry,andtheotherisfive-coordinatedwithadistortedtrigonalbipyramidalgeometry.Themoleculesarepackedintheunitcellintwo-dimensionalnetworkstructurethroughaninteractionbetweentheNatomsofthepyridineandthetinatomsofanadjacentmolecule.
简介:Afacilesyntheticroutetotwoseco-eudesmane,4,5-dioxo-10-epi-4,5-seco-γeudesmane(1)and4,5-dioxo-10-epi-4,5-seco-γ-eudesmol(2)from(+)-dihydrocarvonehasbeendescribed.Avoidingexpensivereagents,thishighlyeconomicmethodespeciallysuitsforthesynthesisof4,5-seco-eudesman-typeandophianon-typesesquiterpeneswithadoublebondatposition11and12.
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:Sixnewcompounds,α,β-KaHb[GeW9M3(H2O)3O37].xH2O(M=Al,Ga,In;a+b=7)andα-K9H5[Ge2W18Ga6(H2O)3O74].20H2O,weresynthesizedfromthelacunaryprecursorsαandβ-GeW9O3410-andcharacterizedbyelementalanalysis,spectroscopyandelectrochemistry.Tungsten-183NMRspectraofthetitlecomplexesconsistoftwolineswithintensityratio2:1asexpectedfortrisubstitutedheteropolyanions.Theintensityratioofα-Gacompoundis1:2,whichisdifferentfromothers(2:1).WiththehelpofFABmassspectrum,weconcludedthatitisadimerwithD3h,structureinaqueous,andtheothersexistbymonomerswithC3cstructures.
简介:Newphosphorus-andselenium-containingheterocyclyes,1,3,2,6-dioxaphosphaselena-cyclooctanes(la-1h),weresynthesizedbythereactionofbis(2-hydroxyethyl)selenidewithRP(X)Cl2whereR=alkoxyl,aroxyl,arylandX=Oorlonepair.Theirstructuresweredeterminedbyspectro-scopiesandelementalanalysesandfinallyconfirmedbytheX-raycrystallographicanalysisof1c.Themolecularstructuresoftheheterocycleswerediscussedintermofconformationalanalysis.
简介:ThetitlecomplexEu(Ⅲ)(TTA)3(phen)(whereTTA=thenoyltrifluoroacetonemonoanion;phen=1,10-phenanthroline)hasbeensynthesizedinmixedsolventsofacetoneandethanol(1:1volumeratio)anditscrystalstructurehasbeendeterminedbyX-raydiffraction.Thecomplexcrystalsaretriclinic,spacegroupP1(#2)withcelldimensionsofa=1.3241(2)nm,6=1.5278(4)nm,c=0.9755(3)nm,α=92.49(2)°,β=102.57(2)°,γ=91.62(2)°,V=1.9268(8)nm3,Z=2,μ(MoKα)=18.77cm-1,Dx=1.720g/cm3.ThecoordinationgeometryofEuatomisadistortedsquareantiprism,andtheencapsulatedstructurethatcanmeetthestructuralrequirementofthetypicaleuropiumluminescentsensor.Thefluorescencespectrumsuggeststhatthecomplexisastrongphotoluminescentmaterial.
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:AsimpleandefficientcascadeMichael/cyclizationreactionof3-aminoindolin-2-oneswithenones/enalswasidentifiedforthesynthesisofpotentiallybiologicallyactive3’,4’-dihydrospiro[pyrrol-3,2’-oxindoles],usingDBUasanefficientcatalystandethyleneglycolasanenvironmentallybenignsolvent.Morediverse3’,4’-dihydrospiro[pyrrol-3,2’-oxindoles]analoglibrarieswerepreparedingoodyields(upto97%).Thestructureof3’,4’-dihydrospiro[pyrrol-3,2’-oxindoles]wasconfirmedbymassspectrometryanalysis,NMRanalysisandsinglecrystalX-raydiffraction.Themainadvantagesofthismethodincludetheavailabilityofstartingmaterials,simpleexperimentaloperation,shortreactiontime,aswellashighyieldsobserved.
简介:ThecomplexK3H4GeW9V3O40·8H2OcrystallizedinamonocliiniesystemwithspacegroupP2,Mr=2784.67,a=11.099(3),b=16.452(4),c=13.534(4),β=108.14°,Z=2,V=2348.493,F(000):2456,μ=239.7cm-1,De=3.932g/cm3.ThefinalR=0.083for4528non-zeroreflexions.ThestructureofanionsGeW9V3O40andGeW9O34belongstoA--type.
简介:Theapplicationof5'-nitrosalicylfluorone(5'-NSF)-molybdenum(Ⅵ)complexasaspectroscopicprobewasstudied.InthebuffermediumofHOAc-NaOAcat3.45andinthepresenceofPVA124microemulsion,5'-NSF-Mo(Ⅵ)complexcombinesproteinrapidlytoformastablecompound,leadingtoanabsorbancedecreaseat525nmof5'-NSF-Mo(Ⅵ)complex.Accordingtothischange,microdeterminationofproteinhasbeendescribed.Bovineserumalbumin(BSA)couldbedeterminedinthelinearrangeof0—16μg·mL^-1withthedetectionlimitof11ng·mL^-1.Manyaminoacidandmetalionsstudieddonotinterferewiththeassay.Themethodpossesseshighsensitivityaswellashighselectivity.Itcanbeusedtodetermineproteininhumanurineandmilkpowdersuccessfully.Therelativestandarddeviationsareinallinstanceslessthan4.7%,andtherecoveriesarebetween97.6%and106.0%.Moreover,thebindingnumberofBSAwiththecomplex,whichisdeterminedbyusingmolarratio,Rosenthanlgraphicandsloperatiomethods,isingoodagreementwitheachother.