为考察取代环戊二烯基或桥联环戊二烯基有机稀土化合物的性质,研究了碳桥联芴基环戊二烯基配体与卤化稀土的反应,其中,[2-(9-芴基)异丙基]环戊二烯基锂[Flu(Me)2CCpLi]与三溴化镱(YbBr3)在四氢呋喃(THF)中反应,分离得到了标题配合物[Flu(Me)2CCp]2Yb(μ-Br)2Li(THF)2·THF.X射线单晶结构测定表明配合物属单斜晶系,空间群为P2(1)/n,晶胞参数为:a=1.4676(3) nm,b=1.2618(4) nm,c=2.9736(9) nm,β=98.172(18)°,Z=4,V=5.451(2) nm3,Mr=1098.84,Dc=1.339 mg·m-3,R=0.0695,wR=0.1721.中心Yb原子分别与两个环戊二烯基和两个溴原子成键,形成扭曲的四面体配位构型.Yb-Br1和Yb-Br2键长分别为0.2765(1)和 0.2738(1) nm,两个环戊二烯基平面的夹角为125.7°,中心Yb原子与两个环戊二烯基环中心的平均距离分别为0.232和0.231 nm.
参考文献
| [1] | Schumann H;Meese-Marktscheffel J A;Esser L .Synthesis,structure,and reactivity of organometallic π-complexes of the rare earths in the oxidation state Ln3+ with aromatic ligands[J].Chemical Reviews,1995,95:865. |
| [2] | 程延祥,金国新.有机希土金属含硫族化合物的研究进展[J].无机化学学报,1999(01):8-18. |
| [3] | Anwander R. ."Self-assembly" in organolanthanide chemistry: Formation of rings and clusters[J].Angewandte Chemie International Edition,1998(5):599-602. |
| [4] | Giardello M A;Yamamota Y;Bard L et al.Stereocontrol in the polymerization of methyl methacrylate mediated by chiral organolanthanide metallocenes[J].Journal of the American Chemical Society,1995,117:3276. |
| [5] | Qian CT.;Sun J.;Nie WL. .C-s-symmetric ansa-lanthanocenes designed for stereospecific polymerization of methyl methacrylate. Synthesis and structural characterization of silylene-bridged fluorenyl cyclopentadienyl lanthanide halides, amides, and hydrocarbyls[J].Organometallics,2000(20):4134-4140. |
| [6] | Qian C T;Nie W L;Sun J.Synthesis of diphenylmethylene bridged fluorenyl cyclopentadienyl lanthanocene complexes with Cs symmetry and crystal structures of the ate complexes[Li(thf)4][LnCl2{(C13H8)CPh2(C5H4)}] and[Li(thf)4][Ln(BH4)2{(C13H8)CPh2(C5H4)}](Ln=Nd or La)[J].Journal of the Chemical Society Dalton Transactions,1999:3283. |
| [7] | 程延祥,金国新,贾恒庆,邢彦,林永华.Synthesis and Crystal Structure of(1,3-tBu2C5H3)2Sm(μ-Cl)2Li(THF)2[J].结构化学,2001(01):31-33. |
| [8] | Hitchcock PB.;Tian S.;Lappert MF. .Lanthanocene chemistry with [Cp-R](-), [Cp-t](-), [Cp-tt](-), and [(Cp2SiMe2)-Si-R '](2-) ligands: Synthesis and characterization of bis(cyclopentadienyl)lanthanide(III) halides and bis(cyclopentadienyl)lanthanide(II) complexes and crystal structures[J].Organometallics,2000(17):3420-3428. |
| [9] | Toylor M D;Carter C P .Preparation of anhydrous lanthanide halides,especially iodides[J].Journal of Radioanalytical and Nuclear Chemistry,1962,24:387. |
| [10] | Razavi A;Ferrara J .Preparation and crystal structures of the complexes(η5-C5H4CMe2η5-C13H8) MCl2(M=Zr,Hf) and their role in the catalytic formation of syndiotactic polypropylene[J].Journal of Organometallic Chemistry,1992,435:299. |
| [11] | Sheldrick G M.SHELXTL97.University of Gttingen[M].Germany,1997 |
| [12] | Siemens.XSCANS.Version 2.10.Siemens Analytical X-ray Instruments Inc[M].Madison,Wisconsin,USA,1994 |
| [13] | Lueken H;Schmitz J;Lamberts W et al.Structural chemistry and magnetism of dicyclopentadienidehalides of lanthanides,part 6,ytterbiumdicyclopentadienidechloride and -bromide,[Yb(C5H5)2Cl]2 and[Yb(C5H5)2Br]2[J].Inorganica Chimica Acta,1989,156:119. |
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