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1、Inorg.Chem.1991,30,609-618609ContributionfromtheDipartimentodiScienzeChimiche,UniversitidiTrieste,34100Trieste,ItalySynthesis,MolecularStructure,andChemicalBehaviorofHydrogentrans-Bis(dimethylsulfoxide)tetrachlororuthenate(111)andmer-Trichlorotris(dimethy1sulfoxide)ru
2、thenium(III):TheFirstFullyCharacterizedChloride-DimethylSulfoxide-Ruthenium(111)ComplexesEnzoAlessio,*GabrieleBalducci,MarioCalligaris,GiacomoCosta,WahibM.Attia,?andGiovanniMestroniReceivedFebruary1.5,I990Thesynthesis,molecularstructureandchemicalbehavioroftwochloride
3、4imethylsulfoxide-ruthenium(II1)derivatives,namely[(DMSO),H][tran~-Ru(DMS0)~Cl~](1)and~~~-RU(DMSO)~CI,(2),arereported.Theyrepresentthefirstexamplesoffullycharacterizedhalogen-dimethylsulfoxide-ruthenium(ll1)complexes.Furtherrelevanceintheirsynthesiscomesfromtheknownmt
4、itumorpropertiesofisostructuralRu(ll1)complexeswithheterocyclicnitrogenligandsandofhalogen-dimethylsulfoxide-ruthcnium(l1)complexesaswell.Thecrystalstructuresof1and2havebeendeterminedbythree-dimensionalX-rayanalyses.Crystaldataareasfollows:[(DMSO),H][trans-R~(DMSO)~Cl
5、,l,monoclinic,spacegroupP2/n,a=9.273(I)A,b=16.509(3)A,c=14.023(3)A,0=100.79(2)O,Z=4,R=0.041;former-Ru(DMS0)3C13,monoclinic,spacegroupP2,/c,a=10.105(2)A,b=13.832(3)A,c=1I.I15(2)A,0=94.39(2)O,Z=4,R=0.028.In1therearetwocrystallographicallyindependent[Ru(DMSO),CI,]-anions
6、lyingoncrystallographic2-foldaxes,passingthroughRuandtwotransC1atoms,sothattheothertwoCIatomsandthetwoS-bondedDMSOmoleculesarealsotranstoeachother.CationsareprovidedbyprotonatedDMSOmolecules,[Me2S0...H...0SMe2]+.In2thethreechlorineatomsareinthemerconfiguration,andthet
7、wotransDMSOmoleculesarcS-bondcdtoRu,whilethethirdoneis0-bonded.Bothcomplexesareintermediatesinthesynthesisofc~~-RuCI,(DMSO)~fromhydratedRuC13.Cyclicvoltammetricevidenceshowsthat,indimethylsulfoxideanddichloromethanesolution,2isincquilibriumwithanisomerthatverylikelydi
8、ffersinthecoordinationmodeofoneDMSO(S-to0-bondedisomerization).Thechcmicalbehaviorof1and2inaqueoussolutionhasbeenstudiedatlo
