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1、第2期1997年6月无机化学学报JOURNALOFINORGANICCHEMISTRYVol.13,No.2June,1997Ξ双脂肪胺钌卟啉的合成、结构表征和晶体结构李早英3(武汉大学化学系,武汉430072)支志明(香港大学化学系,香港)本文讨论了一系列双脂肪胺钌卟啉配合物,包括Ru(II)(Por)(H2NR)2和Ru(II)(Por)(HNR2)2Por=四苯基卟啉(TPP),中位2四(对甲苯基)卟啉(TTP),中位2四(对氯苯基)卟啉(42Cl2TPP);R=叔丁基,异丙基,环己基,正辛基,正十二烷基,R′=甲基和
2、乙基]的合成,结构表征和晶体结构测定。钌羰基卟啉与间2氯过苯甲酸的反应混合物用过量的脂肪胺处理,得到高收率的双脂肪胺钌卟啉配合物。所有的新配合物经核磁共振光谱,红外光谱,紫外光谱以及元素分析得到证实。其中,配合物Ru(II)(Por)(H2NBu2t)2的结构已由X2射线晶体结构测定。在Ru(II)(Por)(H2NBu2t)2分子中,Ru2N(Por)和Ru2N(H2NBu2t)键长分别为21041∼和21175∼。关键词:脂肪胺钌卟啉合成结构表征晶体结构测定BIS(ALIPHATICAMINE)RUTHENIUM(Ⅱ)P
3、ORPHYRINSSYNTHESIS,SPECTROSCOPYANDCRYSTALSTRUCTURELiZaoying3(DepartmentofChemistry,WuhanUniversity,Wuhan430072)CheChiming(DepartmentofChemistry,TheUniversityofHongKong,HongKong)Thesynthesis,characterizationandreactivitiesofaseriesofrutheniumporphyrinsincludingRuⅡ(P
4、or)(H2NR)2andRuⅡ(Por)(HNR2)2Por=tetraphenylporphyrinato(TPP),meso2tetrakis(p2tolyl)porphyrinato(TTP),meso2tetrakis(42chlorophenyl)porphyrinato(42Cl2TPP);R=tert2butyl,isopropyl,cyclohexyl,n2octyl,n2dodecyl,R′=methyl,ethylaredescribed.ThereactionofRu(Por)(CO)(MeOH)wi
5、thm2chloroperoxylbenzoicacid(m2CPBA)followedbytreatmentofthereactionmixturewithexcessaliphaticaminesreadilygavebis(aliphaticamine)ruthenium(Ⅱ)por2phyrinsinhighyields.Allthenewcomplexeshavebeencharacterizedby1HNMR,IR,andUV2Visiblespectroscopy.TheX2raycrystalstructur
6、eofRu(TTP)(H2NBut)2hasΞReceived:1996205214.Revised:1996210215.3LiZaoying,female,inJuly1949,associateprofessor,currentresearchinterestisinthestudyonsynthesisandpropertiesofmacrocyclicpolyamineandmetalcomplexes.beendetermined.TheRu2N(Por)andRu2N(H2NBut)(H2NBut)2are0.
7、2041nmand0.2175nm,respectively.distancesinRu(TTP)character2Keywords:izeationaliphaticaminerutheniumporphyrinsynthesis0IntroductionAlthoughthechemistryoftransitionmetalaminecomplexeshasbeenintensivelystudied,relativelyfewreportshavebeenmadeonthebis(amine)adductsofme
8、talloporphyrins,andsuchreportshavemainlyconcentratedonaromaticaminesaxialligands,suchaspyridineandimida2zole1.Thefirstbis(aliphaticamine)metallop
