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Synthesis and Structure of an Enantiopure Dirhodium Loop with Unusual Axial Coordination.pdf
3O卷 6期 结 构 化 学 (胱 0厂【觎： 旧) Vo1．30，No．6
2011．6 Chinese Struct． Chem． 892～896
SynthesisandStructureofanEnantiopure
Dirhodium LoopwithUnusualAxialCoordination①
CHEN Jin YU Rong．Min MURILLOCarlosAb
(StateKeyLaboratoryofStructuralChemistry,FujianInstituteofResearchonthe
StructureofMatter,ChineseAcademyofSciences，Fuzhou,Fujian35002，China)
(DepartmentofChemistry,TexasAMUniversity,POBox30012,
CollegeStation,TX,77842—3012，UnitedStatesofAmerica)
ABSTRACT nlecrystalsofen_antiopureSS-[cis-Rh2(Ph2C6H4)2(O2CC2F4CO：)!]2((CH3)2CHCH2NH2)3
(1) were obtained from the reaction of S-[cis-Rh2(Ph2C6H4)2(CH3CN)6]BF4 (S-2) and
(Et4N)2(O2CC2F4CO21inCH2CI2／CH3OHunderthepresenceofsec-butylamine．Compound1
crysatllizesinorthorhombic，spacegroupP2a2121witha=16．880(5)，b=28．728(9)，c=20．475(6)A，
=9929(5)A，z=4，C95H96CIsFsN3Os
． 5oP4Rh4，Mr=2280．52，Dc=1．526g／cm，F(ooo)=4608and
la(MoKa)=0．922mm-．ThefinalR=0．0488andwR；0．1164for17204observedreflectionswithI
2o(0andR=0．0814andwR=0．1374foralldaatwithabsolutestructureparameter：一0．04(3)．
Compound1containstwoinherentlychiralS-[cis—Rh2(Ph2C6H4)2]moietieswhichareconnectedby
wto(O2CC2F4CO2)dicarboxylateligandsintheequatorialpositions．Oneofthedirhodiumunitswith
Rh-Rhdistanceof2．5445(8)Aisfurthercoordinatedbyasec．butylamineineachaxialposition．
Anotherdirohdium unithasonly one axialsee-butylamineligand，and itsRh-Rh distanceis
2．5079(9)A．
Keywords：enantiopure，chiral，dirhodium，orthometalated，crystalstructure
1 INTRODUCTION cisoidorthometalated phosphinesin ahead．．to．．atil
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