Chen-2004-Europium(II) and ytt

化学文献。硼氢化镁

Europium(II)andYtterbium(II)CyclicOrganohydroborates:AnEuropium(II)ComplexwithanAgosticInteraction

XuenianChen,SoyoungLim,ChristineE.Plecˇnik,ShengmingLiu,BinDu,EdwardA.Meyers,andSheldonG.Shore*

DepartmentofChemistry,TheOhioStateUniVersity,Columbus,Ohio43210

ReceivedAugust7,2003

Lanthanidebis((cyclooctane-1,5-diyl)dihydroborate)complexes(THF)4Ln{(µ-H)2BC8H14}2(Ln)Eu,1;Yb,2)weresynthesizedbyametathesisreactionbetween(THF)xLnCl2andK[H2BC8H14]inTHFina1:2molarratio.Attemptstopreparethemonosubstitutedlanthanidecyclicorganohydroborates(THF)xLnCl{(µ-H)2BC8H14}wereunsuccessful.OnthebasisofthemolecularstructureandIRspectrumof1,thereisanagosticinteractionbetweenEu(II)andoneoftheR-C Hhydrogensfromthe{(µ-H)2BC8H14}unit.Nosuchinteractionwasobservedfor2.ThecoordinatedTHFin1and2canberemovedunderdynamicvacuum,butthesolventligandsremainboundtoYbwhen2isdirectlydissolvedinEt2Oortoluene.InstrongLewisbasicsolvents,suchaspyridineorCH3CN,attackoftheYb H http://www.wendangxiazai.compound2wasreactedwith2equivofthehydrideionabstractingreagentB(C6F5)3toaffordthesolvent-separatedionpair[Yb(THF)6][HB(C6F5)3]2(3).Complexes1,2,and3werecharacterizedbysingle-crystalX-raydiffractionanalysis.Crystaldata:1isorthorhombic,Pna21,a)21.975(1)Å,b)9.310(1)Å,c)16.816(1)Å,Z)4;2istriclinic,P1h,a)9.862(1)Å,b)10.227(1)Å,c)10.476(1)Å,R)69.87(1)°, )76.63(1)°,γ)66.12(1)°,Z)1;3 Et2Oistriclinic,P1h,a)13.708(1)Å,b)14.946(1)Å,c)17.177(1)Å,R)81.01(1)°, )88.32(1)°,γ)88.54(1)°,Z)2.

Introduction

Thoughallthelanthanidescanexistinthedivalentstateincrystalline,alkalineearthmetalhalidelattices,onlySm(II),Eu(II),andYb(II)arereadilyaccessibleundernormalreactionconditions.1,2Thefirstdivalentlanthanidemetal-lacarboranecomplex,[Yb(C2B9H11)(DMF)4],wasreportedbyHawthorneandco-workers.3Shortlythereafter,ourlaboratorypreparedaytterbium(II)decaboratecompound,(CH3CN)6Yb{(µ-H)2B10H12} 2CH3CN,inwhichthe[B10H14]2-unitcoordinatestoYb(II)throughtwoYb-H-Bbridgebonds.4Inadditiontothisworkonpolyhedralboronhydrides,abundantstudiesonLn(III)tetrahydroborateshave

*Towhomcorrespondenceshouldbeaddressed.E-mail:shore@chemistry.ohio-state.edu.

(1)McClure,D.S.;Kiss,Z.

Chen-2004-Europium(II) and ytt

J.Chem.Phys.1963,39,3251.

(2)Evans,W.J.;Allen,N.T.;Workman,P.S.;Meyer,J.C.Inorg.Chem.

2003,42,3097.

(3)Manning,M.J.;Knobler,C.B.;Hawthorne,M.F.J.Am.Chem.Soc.

1988,110,4458.

(4)(a)White,J.P.,III;Deng,H.;Shore,S.G.J.Am.Chem.Soc.1989,

111,8946.(b)White,J.P.,III;Shore,S.G.Inorg.Chem.1992,31,2756.

beenreported.5However,therearefewreportsondivalentlanthanide[BH4]-systems,6andtothebestofourknowl-edge,nosyntheticstudieshavebeenpublishedonlanthanide-(II)organohydroborates.ItisworthyofnotethatZanellaetal.7characterizedthefirstactinideorganohydroborateCp3U{(µ-H)2BC8H14}thatincorporatesthe[H2BC8H14]-ligand,theorganohydroborateanionofthe9-BBNdimer.8

Recently,wesynthesizedaseriesofgroup4and5metallocenecyclicorganohydroboratesystemscontainingthe[H2BC4H8]-,[H2BC5H10]-,and[H2BC8H14]-ligands.9SomeofthesecomplexesexhibitunusualreactivitywithB(C6F5)3toaffordcationicorneutralproductsaccordingtothesolvent’scoordinatingability.10,11Inanefforttoextenddivalentlanthanideborohydridechemistry,theorganohy-(5)(a)Marks,T.J.;Kolb,J.R.Chem.ReV.1977,77,263.(b)Makhaev,

V.D.Russ.Chem.ReV.2000,69,727.

(6)(a)White,J.P.,III;Deng,H.;Shore,S.G.Inorg.Chem.1991,30,

2337.(b)Makhaev,V.D.;Borisov,A.P.Z.Neorgan.Khim.1999,44,1489.

(7)Zanella,P.;Ossola,F.;Porchia,M.;Rossetto,G.;Chiesi-Villa,A.;

Guastini,http://www.wendangxiazai.comanomet.Chem.1987,323,295.(8)(a)Ko¨ster,R.;Seidel,G.Inorg.Chem.1983,22,198.(b)Brown,H.

C.;Singaram,B.;Mathew,http://www.wendangxiazai.com.Chem.1981,46,2712.

692InorganicChemistry,Vol.43,No.2,2004

10.1021/ic030249sCCC:$27.50©2004AmericanChemicalSociety

PublishedonWeb12/13/2003

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