简介:Thecopper(Ⅱ)complex[Cu3(nta)2(azpy)2(H2O2)]·6H2O(nta=nitrilotriacetate,azpy=4,4′-azobispyridine)hasbeensynthesizedandcharacterized.TheX-rayanalysisrevealsthattherearetwokindsofcopper(Ⅱ)coordinationenvironments.Cu(1)hasadistortedsquareplanesymmetryandCu(2)hasadistortedoctahedralsymmetry.Cu(1)islinkedtoCu(2)throughntaandboundtoCu(1C)byazpy,andCu(2)islinkedtoCu(2A)throughazpy,whichextendstotwo-dimensionalnetworkwithlargerhombus1.2nm×1.7nm.
简介:Anovelaciddyeacidwassynthesizedbythecondensationreactionbetweenbromamineacidand2-amino-6-nitrobenzothiazoleanditsanti-UVprotectionpropertieswereevaluated.Theresultsshowedthatsilkdyedwiththisdyehadverygoodultravioletradiationprotectioncapabilityandexcellentdyeingperformance.TheUV-absorptionmechanismofthisdyewasalsodiscussed.
简介:Theneworganic-inorganiccompound,[C_6H_7N_2O_2]_3TeCl_5·2Clwassynthesizedanditsstructurewasdeterminedatroomtemperatureinthetriclinicsystem(P~-1)withthefollowingparameters:a=10.5330(11)?,b=10.6663(11)?,c=15.9751(16)?,α=82.090(2)°,β=71.193(2)°,γ=68.284(2)°andZ=2.ThefinalcycleofrefinementledtoR=0.057andRw=0.149.ThecrystalstructurewasstabilizedbyanextensivenetworkofN--H···Clandnon-classicalC--H···Clhydrogenbondsbetweenthecationandtheanionicgroup.Severalthermalanalysistechniquessuchasthermogravimetricanalysis,differentialscanningcalorimetricanalysisandevolvedgasanalysiswereused.Weusedisoconversionalkineticsmethodstodeterminethekineticsparameters.Weobservethatthedecompositionof[C_6H_7N_2O_2]_3TeCl_5·2Clentailstheformationhydrochloricacidofnitroanilineasvolatiles.Theinfraredspectrawererecordedinthe4000–400cm~(-1)frequencyregion.TheRamanspectrawererecordedintheexternalregionoftheanionicsublatticevibration50–1500cm~(-1).TheopticalbandgapwascalculatedfromtheUV-VisabsorbancespectrausingclassicalTaucrelationwhichwasfoundtobe3.12and3.67eV.
简介:建立了自动消解仪消解-电感耦合等离子体原子发射光谱法(ICP-OES)同时测定水系沉积物中Cu,Zn,Ni,Cr,Pb,Co6种元素含量的方法.方法中6种元素的检出限为0.0002~0.02mg/L,工作曲线的相关系数均大于0.999.方法经国家标准物质(GBW07361)验证,准确度和精密度均能达到环境监测分析的要求,为水系沉积物中重金属元素含量的测定提供了简单可靠的分析方法.
简介:3-(2-Hydroxyphenyl)-6-(4-nitrophenyl)-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine,C16H11N5O3S,waspreparedbythecyclizationof3-(2-hydroxyphenyl)-4-amino-5-mercapto-1,2,4-triazolewith2-bromo-4-nitroacetophenone.Thecompoundwascharacterizedbymeansofelementalanalysis,IR,1HNMR,13CNMR,massspectrometry,andX-raydiffraction.ThecompoundcrystallizesinamonoclinicsystemwithspacegroupCc,a=2.1853(4)nm,b=2.1192(5)nm,c=1.3526(3)nm,β=95.21(2)°,V=6.238(2)nm3,Dcalcd.=1.505Mg/m3,Z=16,F(000)=2916,R1=0.0501,wR2=0.0427.Acomparisonbetweenthecrystalstructuresof1,2,4-triazolo[3,4-b][1,3,4]thiadiazineand1,2,4-triazolo[3,4-b][1,3,4]thiadiazolewasmadeinthestructuralview.Atwo-dimensionalnetworkisformedbyhydrogenbondsandπ-πstackinginteractions.
简介:Ionothermalsynthesiswasusedtoprepareanovelaminoacidcontaininghybridzincophosphatemonomer,[Zn(HPO4)(H2PO4)][C6H10N3O2](denotedasZnPO-CJ58).Theinorganicframeworkof[Zn(HPO4)(H2PO4)]·[C6H10N3O2]consistsof4-memberedringsformedbyZnO3OHisandPO2(OH)2tetrahedra.TheHPO4andaminoacidmoietieshangontheZncenter.Suchaframeworkisstabilizedbyextensivemultipointhydrogenbondsinvolvingthephosphateunitsandhistidinemoleculestoformapseudo-3Dsupramolecularstructure.ItisnoteworthythatZnPO-CJ58isthefirstzincphosphateclusterwithaminoacidactingastheligand.Itexhibitsphotoluminescenceexcitedatawavelengthof220nm.Interestingly,ZnPO-CJ58cantransformintoalayeredstructure(C6H10N3O2)Zn2·(HPO4)(PO4)·H2O(ZnPO-CJ36)throughfurtherreactingwithwaterorzincacetatedihydrateinwaterat85℃for1h.Thisworkwillbehelpfulforthesynthesisofcrystallineinorganic-organichybridmaterialswithbiofunctionalmolecules.
简介:利用水热合成方法合成了2个新的双核稀土-异烟酸配合物修饰的Dawson型有机-无机杂化化合物[Ln2(HINC)4(H2O)8(P2W18O62)]·nH2O(Ln=Ce(1),Eu(2);n=16(1),9(2);INC=4-吡啶羧酸/异烟酸).化合物1与2同构,并通过红外光谱、元素分析和X-射线单晶衍射方法确定了该化合物的晶体结构.单晶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=1.3236(3)nm,b=1.8650(4)nm,c=2.2872(5)nm,α=67.26(3)°,β=78.01(3)°,γ=70.34(3)°,V=4.8838(17)nm3,Z=2.化合物2也属于三斜晶系,P-1空间群,晶胞参数a=1.3201(2)nm,b=1.8569(3)nm,c=2.2856(4)nm,α=67.378(2)°,β=77.745(3)°,γ=70.039(3)°,V=4.8398(13)nm3,Z=2.
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:8,8′-Dibromo-6,6′,7,7′-tetramethoxy-5,5′-diisopropyl-3,3′-oxydimethylenedinaphtho[2,1-b:2′,1′-d]furan,C32H30Br2O;M.W.=670;triclinic;spacegroupP1;a=8.896(2),b=10.216(1),c=10.423(1)A,α=108.48(1),β=119.36(1),γ=99.26(1);V=723.5A3;Z=1,Dcal.=1.479g.cm-3.MoKα=28.11cm-1,F(000)=326,T=293K.Thestructurewassolvedbydirectmethodandfull-matrixleast-squaresrefinementconvergedatR=0.034for2377observedreflections.Theoxygenatominseven-memberedringexistsinadisorderedarrangement.Bothbisnaphthaleneandoxygen-containingfive-memberedringhaveplanarconformationswithdihedralangle6°,showingmarkedaromaticfeature.
简介:Themononuclearcomplex,[NtCl2(trzCHzCHzCOPh)4]·6H2O(trz=1,2,4-triazole),wassynthesizedanditsstructurewasdeterminedbysinglecrystalX-raydetermination.Itcrystallizesinthemonoclinicsystem,spacegroupP21/c,withlatticepa-rameters:a=0.80391(2)nm,b=1.06215(2)nm,c=2.90133(2)nm,β=94.792(1)°andZ=2.EachnickelatomiscoordinatedbyfourNatomsoftriazolefromfourβ-(1,2,4-IriHole-1-yl)propiophenoneligandsandtwochlorideanionsinarrangementwithoctahedralcoordinationgeometry.Inadditiontothecoordinatingnickelcomplex,therearesixunco-ordinatedwatermolecules.TheNi—Ndistanceis0.24865(8)nmandtheNi—Ndistaneesareintherangeof0.2072(2)to0.2099(2)nm,respectively.Inthesolidstate,theUtiecom-poundformsthreedimensionalnetworkstructurethroughhy-drogenbonds.Theintermolecularhydrogenbondsconnectthe[NiCl2(C2H2N3CH2CH2COPh)4]andH2Omoieties.Thedeepgreencrystalswerealsoexaminedbyelementalanalysis,FT-IRandUVspectra,whichareinagreementwiththestructuralda-ta.
简介:通过水热法合成了一维链状的磷钼氧酸盐(DETA)。NaNa(H5P4Mo6O31)2]·8H2O(DETA—Diethylenetriamine),采用x-射线单品衍射结构分析,元素分析和红外光谱等表征.该磷钼氧酸盐属于三斜晶系,空间群是P-1,晶胞参数a=1.2434(3)nm,6—1.2610(3)nm,c=1.3079(3)nm,a=85.418(3)°,β=73.399(2)°),γ=82.175(3)°,V=1.9450(8)Elm。,F(000)=1462,Z=:=2.标题化合物的结构是由Na(H5P4Mo6O31)2簇单元,二亚乙基三胺阳离子和结晶水分子组成.另外,Na(H5P4Mo6O31)2簇由钠离子连接形成了一维的链结构.一维链结构又由于二亚乙基三胺阳离子和结晶水分子形成的氢键进一步连接三维超分子结构.用标题化合物修饰的碳糊电极(APM—CPE)对AA氧化有很好的电催化活性.
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.
简介:利用L-脯氨酸催化的5-氯水杨醛(1)与6-甲基-4-羟基吡喃酮(2)的缩合反应及硫酸铜催化下与1,3-二甲基-5-氨基吡唑(3)的串联反应,合成得到了10-氯-1,3-二甲基-5-(2-氧代丙基)色烯并[4,3-d]吡唑并[3,4-b]吡啶-6(3H)-酮(4)和10-氯-5-二乙氧基甲基-1,3-二甲基色烯并[4,3-d]吡唑并[3,4-b]吡啶-6(3H)-酮(5).化合物5的结构通过单晶X射线衍射法确定:晶体属于三斜晶系,空间群P-1;相对分子质量Mr=803.68;晶胞参数a=1.03160(10)nm,b=1.42900(13)nm,c=1.44268(15)nm;V=1.9448(3)nm~3;Z=2;晶胞密度Dc=1.372g/cm~3;吸收系数μ=0.228mm-1;单胞中电子的数目F(000)=840.晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R=0.0681,wR=0.2051.在晶体结构中色烯环与吡啶环及吡唑环近似于共平面.
简介:标题化合物(C30H35N3)以4-甲基苯甲醛、环十二酮和3-甲基-1-苯基-1H-吡唑-5-胺,在三氟乙酸和醋酸的作用下,经微波辐射合成得到.其结构通过单晶X射线衍射法确定,晶体属单斜晶系,空间群P21/c,相对分子质量Mr=437.61,晶胞参数a=1.08926(11)nm,b=2.1927(2)nm,c=1.04954(14)nm,V=2.4641(5)nm3,Z=4,晶胞密度Dc=1.180g/m3,吸收系数μ=0.069mm-1,单胞中电子的数目F(000)=944.晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R=0.0468,ωR=0.0905.在晶体结构中新形成的吡啶环为共平面结构.