Hydrothermal synthesis and characterization of.pdf

Hydrothermal synthesis and characterization of.pdf

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1、Cryst.Res.Technol.42,No.10,955–960(2007)/DOI10.1002/crat.200710924Hydrothermalsynthesisandcharacterizationof(N(C2H5)4)4[VMo12V2O44]11123S.Cevik*,Z.Alkan,M.Poyraz,M.Sar?,andO.Büyükgüng?r1DepartmentofChemistry,ScienceandLiteratureFaculty,AfyonKocatepeUniversi

2、ty,AfyonkarahisarTR-03200,Turkey2DepartmentofPhysicsEducation,EducationFaculty,GaziUniversity,Be?evler-AnkaraTR-06500,Turkey3DepartmentofPhysics,ScienceandLiteratureFaculty,OndokuzMay?sUniversity,Kurupelit-SamsunTR-55139,TurkeyReceived23February2007,revised

3、19April2007,accepted26April2007Publishedonline12June2007Keywordspolyoxometalate,heteropolyoxometalate,polyoxomolybdate,heteropolyoxomolybdate,heteropolymolybdovanadate.PACS61.66.FnThehydrothermalreactionofamixtureofNa2MoO4·2H2O,V2O5,pyromelliticacid(1,2,4,5

4、-C6H2(COOH)4),IV(C2H5)4NCland0,1MH2SO4for88hat180°Cgivesblueneedle-likecrystalsof[V2O2(H2O)2(C6H2(COO)4)]in20%yield(basedonV)anddarkblueprismaticcrystalsofthetitlecompound,mixed-valance(N(C2H5)4)4[VMo12V2O44],1,in12%yield(basedonMo).1wasinvestigatedbymeanso

5、felementalanalysis,thermogravimetry,FourierTransformInfraredSpectroscopyandSingleCrystalX-rayDiffractionMethods.Crystaldataforthecompound:monoclinicspacegroupP21/c(No:14),a=13.7815(12)-nb=13.0271(9)c=21.189(2)?,β=113.909(7)°,Z=2.Although[XM14O42](X=P,Si,Ge,

6、VandM=Mo-4and/orV)coreshavebeenpreviouslydetermined,thisisthefirsttimethat[VMo12V2O44]coreissynthesizedandcharacterized.Thestructuraldifferencebetween1andtheseHPOMsisthecoordinationalgeometryofthecentralmetalatoms.Thecentralvanadiumin1hasanoctahedralcoordin

7、ationgeometry,-9-4-5whereasinliterature,thecentralV,P,SiandGeatomsin[V15O42]/[SiM8V6O42]/[PM8V6O42]/-4[GeM8V6O42]havetetrahedralcoordinationalgeometry.?2007WILEY-VCHVerlagGmbH&Co.KGaA,Weinheim1IntroductionHeteropolyoxometalates(HPOMs)haveattractedanextensiv

8、einterestinthecontemporarymaterialchemistryowingtothewiderangeofdifferentstructuralcharacteristicsandpotentialcatalytic,photochemical,electrochromicalandmagneticapplicationsinrecentyears[1-5].Therefore

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