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钴(Ⅲ)配合物［Co(NH3)4(N3)2］ClO4晶体结构及其激光化学感度.pdf5页
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第 １７卷　第６期 含　能　材　料 Ｖｏｌ．１７，Ｎｏ．６
２００９年 １２月 ＣＨＩＮＥＳＥＪＯＵＲＮＡＬＯＦＥＮＥＲＧＥＴＩＣＭＡＴＥＲＩＡＬＳ Ｄｅｃｅｍｂｅｒ，２００９
文章编号：１００６玻梗梗矗保ǎ玻埃埃梗０６玻埃叮梗椽玻埃 钴（ ）配合物［Ｃｏ（ＮＨ ）（Ｎ ）］ＣｌＯ Ⅲ ３ ４ ３ ２ ４ 晶体结构及激光化学感度 盛涤伦，马凤娥，张裕峰，朱雅红，陈利魁，杨　斌 （陕西应用物理化学研究所，陕西 西安 ７１００６１） 摘要：制备了高氯酸 ?四氨 ?双叠氮基合钴（ ）（ＤＡＣＰ）的单晶，用Ｘ玻颍幔单晶面探衍射仪测定了其晶体结构。结果 Ⅲ 表明，晶体属三斜晶系，空间群为 Ｐ玻薄＞体学参数为：ａ＝０．７４２２９（９）ｎｍ， ＝９３．２４４（２）°；ｂ＝１．２１２７３（１４）ｎｍ， α ３ ＝１００．０７４（２）°；ｃ＝１．８１２４（２）ｎｍ， ＝９８．０３３（２）°。晶胞体积 Ｖ＝１．５８５１（３）ｎｍ，晶胞分子数 Ｚ＝６，计算密度 β γ 玻 玻 Ｄ ＝１．９５２ｍｇ?ｍｍ ，线性吸收系数 ＝１．９０１ｍｍ ，单胞中电子数目Ｆ（０００）＝９４８。该化合物对６３５ｎｍ的激光非常敏感。 Ｃ μ 关键词：物理化学；钴（ ）配合物；晶体结构；激光化学感度 Ⅲ 中图分类号：ＴＪ５５；Ｏ６４ 文献标识码：Ａ ＤＯＩ：１０．３９６９／ｊ．ｉｓｓｎ．１００６玻梗梗矗保２００９．０６．０１３ 制备了ＤＡＣＰ的单晶，测定了晶体结构，并研究了它的
１　引　言 激光化学感度。 钴氨配位化合物含能材料的研究近年来一直比较 ２　实验部分
活跃。典型代表有：高氯酸 ?五氨 ?（５睬杌四唑）合
钴（ ［１－２］ ２．
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联苯甲酸配位聚合物的合成、结构及性质研究
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硫自由基与不饱和体系的选择性反应研究,自由基与疾病,自由基与衰老,自由基与癌症,自由基与大气,自由基与酶,自由基与健康,自由基与人类健康,自由基与衰老的关系,自由基与疾病的关系
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CatalysisToday133–135(3
SynthesisandcharacterizationoftitaniumketimidecomplexesTi(NCtBu2)nCl4?n(n=1,2):Ethylenepolymerizationstudies
^sMatos,M.TeresaDuarte,M.Merce^sMarques,AnaM.Martins*~oFerreira,IneM.Joa
?micaEstrutural,InstitutoSuperiorTe?cnico,Av.RoviscoPais,1,Lisboa,PortugalCentrodeQu?
Availableonline30January2008
Compounds[Ti(NCB
CBCBCBCBCBC
CR1R2)Me]+,
whichareacceptedastheactivespeciesinolefinpolymeriza-
tioncatalysis,havebeenstudiedbyPiersetal.[27,28].
Wehaverecentlyreportedthatthetitaniumtris(ketimide)
complexTi(NCB
*Correspondingauthor.Tel.:+;fax:+.
E-mailaddress:ana.martins@ist.utl.pt(A.M.Martins).
/$–seefrontmatter#2007ElsevierB.V.Allrightsreserved.
doi:10.1016/j.cattod.
~oFerreiraetal./CatalysisToday133–135(3M.Joa
H,13C,19F,and11BNMRspectrawererecordedinaVarian
Unity300,at298Kunlessstatedotherwise.1Hand13CNMRspectrawerereferencedinternallytoresidualprotio-solvent(1H)orsolvent(13C)resonancesandreportedrelativetotetramethylsilane(d0).19Fand11BspectrawerereferencedexternallytoCF3COOH(d?76ppm)andBF3?Et2O,respec-tively.PeakassignmentswereaidedbyNOEexperiments(one-andtwo-dimensional)andbyonebond13C–1Hhetero–correlations,asappropriate.1HNMRand13CNMRpolymerspectrawereobtainedonsamplesdissolvedineitheramixtureof1,3,5-trichlorobenzenewith30%C6D6at1108C(thespectrawerereferencedinternallyusinghexamethyldisiloxanedH0.058,dC1.9relativetotetramethylsilane,TMS)orCDCl3atroomtemperature.
High-resolutionelectronionisation(EI)massspectrawereobtainedbyaFouriertransformioncyclotronresonancemassspectrometer(FinneganFT/MS2001-DTspectrometer),equippedwitha3-Tsuperconductingmagnet.FAB/MSspectrawereobtainedinaTRIO2000,VGMicromassSpectrometerattheUniversityofRoueninFrance.Elementalanalyseswere
obtainedfromtheLaborato
?riodeAna?lisesdoIST(FisonsInstrument1108).
ClMgCH2Ph(1.5moldm?3inether)waspurchasedfromAldrichandLiMe(1.8Minether)waspurchasedfromMerk.Bothweretitratedbyusualmethodsbeforeuse.MAO(5%Alintoluene)waspurchasedfromAkzoNobelandusedasreceived.ThecompoundsLiNCBCCtBu2)3Cl,3[29],Ti(NCt
Bu2)4,4[29]andB(C6F5)3
[33]werepreparedaccordingtoliteraturemethods.2.1.[Ti(NCB
CBCB),51.1
(CA(CH3)3),42.2(CB(CH3)3),30.0(C(CAH3)3),28.8(C(t
CBH3)3).1HNMR(C6D5Br,300MHz):1.79(s,18H,BuA),1.52(s,B18H,tBuB).13C-{1H}NMR(C6D5Br,75MHz):208.2A(NC),51.6(C(CAH3)3),42.3(CB(CH3)3),30.0(C(CH3)3),28.0(C(CBH3)3).EI/FTICR-MS:292.)([C9H18Cl3N48Ti]?).MS(FAB,m/z):574(M+?Me),532(M+?tBu).Elem.Anal.Calcd.forC9H184Cl3Ti:C,36.71;H,6.16;N,4.76.Found:C,37.01;H,6.83;N,4.69.2.2.[Ti(NCB
(C(CH3)3),30.3(C(CH3)3).HREI/FTICR-MS:398.)([C18H36Cl2N248Ti]?).Elem.Anal.Calcd.forC18H36Cl2N2Ti:C,54.14;H,9.09;N,7.02.Found:C,53.66;H,10.04;N,6.59.
2.3.Ti(NCtBu2)(CH2Ph)3(3)
1(0.mmol)wasdissolvedin40mLofhexaneandcooledto?508C.ClMgCH2Ph(1.5M,1.5mmol)wasaddedandthemixturewasallowedtoreachroomtemperature.Themixturewasfilteredandthesolventwasremoved.Theresiduewasreextractedinhexane.Pumpingoffthesolventafforded0.138gofadark3redoil(91%yield).1HNMR(C6D6,3003
MHz):d7.12(t,JHmHp=7.2Hz,6H,Hm),6.96(t,JHmHp=7.2Hz,3H,Hp),6.44(d,3JHmHo=7.5Hz,6H,Ho),2.67(s,6H,CH2),1.11(s,18H,tBu).13C-{1H}NMR(C6D6,75MHz):d143.7(Cipso),129.3(Cm),128.8(Co),123.6(Cp),87.5(CH2),47.2(C(CH3)3),30.748(C(CH3)3).HREI/FTICR-MS:461.)([C30H39NTi]?).Elem.Anal.Calcd.forC30H39NTi:C,78.07;H,8.52;N,3.03.Found:C,71.98;H,8.09;N,3.26.2.4.Ti(NCB
CtBu2)(CH2Ph)2(m-CH2Ph)B(C6F5)3](5)
Compound5(0.015g,0.03mmol)wasdissolvedin0.3mLoftoluene-d8andplacedinasealableNMRtube.Thesolutionwasdegassedandfrozenpriortotheintroductionof0.3mLofasolutionofB(C6F5)3(0.017g,0.03mmol)intoluene-d8,thatwasimmediatelyfrozen.Thetubewassealedundervacuumandwasunfrozeninabathat?808C,priortoitsintroductionintheNMRmachine,whereitwasallowedtocometoroomtemperature,asitwasmonitored.Reactionwascompleteinstantlyat?808C,inquantitativeyield.1HNMR(C7D8,?308C,300MHz):d7.4–6.8(m,6H,H9+H10),6.55(d,J=7.8Hz,4H,H8),6.48(m,2H,H3),6.10(t,3JH4H5=6.8Hz,1H,H5),5.95(t,3JH4H5=6.8Hz,2H,H4),3.02(br,s,2H,BCHt
2),2.34(dd,4H,2JHH=10.7Hz,Ti–CH2),1.02(s,18H,Bu).19FNMR(C7D8,?308C,282MHz):d?128.2(s,2F,Fo),?157.7(br,1F,Fp),?162.0(br,2F,Fm).11BNMR(C7D8,?308C,96MHz):d?7.6(s).13C-{1H}NMR(C7D8,?408C,
~oFerreiraetal./CatalysisToday133–135(3M.Joa649
75MHz):d49.6(Ti–CH2),38.5(C(CH3)3),29.8(CH3),29.7
(BCH2,br).
2.6.[Ti(NCt
Bu2)2(CH2Ph)(m-CH2Ph)B(C6F5)3](6)Theprocedureisthesameasdescribedfor5.1HNMR(C7D8,?308C,300MHz):d7.08(d,3JH3H4=7.8Hz,2H,H3),6.883
(t,3JH5H4=6.8Hz,1H,H5),6.78(m,2H,H4),6.50(d,JH8H9=7.5Hz,2H,H8),5.86(m,2H,H9),5.62(m,1H,H10),3.30(s,2H,H6),2.46(s,2H,H1),0.99(s,36H,tBu).19FNMR(C3
7D8,?308C,282MHz):d?123.93(s,2F,Fo),?154.3(t,JFpFm=20.7Hz,1F,Fp),?158.2(t,J11
FpFm=18.3Hz,2F,Fm).BNMR(C7D8,?308C,96MHz):d?7.5(s).13C-{1H}NMR(C7D8,?408C,75MHz):d204.8(NC)
CtBu2((i)inScheme1)[41,42].Thisreaction,however,didnotleadtothetargetcomplexbutto[Ti(NCtBu2)3Cl][29].Althoughsurprising,thisresulthasanalogytoreportsonnon-stoichiometricGroup4metalhalidemetathesisreactionswithlithiumamides[43–45].TheelectrophilicattackwithTMSCl
Crystallographicdatafor2EmpiricalformulaC36H72Cl4N4Ti2Formulaweight798.58Temperature(K)
293(2)Wavelength(A
?)0.70169CrystalsystemTriclinicoSpacegroupP-1
a(A?)12.089(4)b(A?)14.530(6)c(A?)14.693(3)a(8)65.65(3)b(8)79.87(2)g(8)79.28(3)V(A?3))Z
2Dc(gcm?3)
1.155Absorptioncoefficient0.607F(000)856
Crystalsize
0.44?0.10?0.02CrystalmorphologyNeedleColor
urangefordatacollection1.708–24.948
Limitingindices
?14 h 14;?17 k 15;?17 l 0Reflectionscollected/unique[Rint=0.0253]Completenesstotheta99.0%(u=24.948)
Refinementmethod
Fullmatrixleast-squaresonF2Data/restrains/parametersGoodnessoffitonF2
FinalRindices[I&2s(I)]R1=0.0766,wR2=0.1811Rindices(alldata)R1=0.1242,wR2=0.2038Extinctioncoefficient
Largestdiff.peakandhole
0.738and?0.971eA
??3andthetransmetallationreactionbetweenTiCl4and
CtBu2)4isrecoveredattheendofthereaction.Athirdattempttoobtain[Ti(NCtBu2)2Cl2]wasthereactionofTiCl4withtwoequivalentsofasofterketimidetransferreagent,Me3SiNCtB
CBu2)Cl3]2,1,asabrightgreensolid.The
Hand13CNMRspectraof1inthetemperaturerangeof?30to1108Cshowtwosetsofsignalsfortheketimideligand.Thisresultsuggeststhat1isadimerwherethemetalsarepentacoordinatedbytwobridgingchlorideligands,twoterminalchloridesandoneketimideligand.TheNMRdatareflectthustheexistenceoftwoisomericstructuresinsolution,resultingfromdifferentarrangementsoftheketimideligandinthemetalcoordinationsphere.ThisassumptionissupportedbytheFAB/MSspectrumthatshowsonesignalatm/z574correspondingtothedimerparent-ionminusonemethylgroup([M?Me]+).Furtherconfirmationwasattemptedbyhighresolutionmassspectrometry(HREI/FTICR-MS)but
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