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1、JournalofStructuralChemistry,Vol.43,No.2,pp.369-372,2002OriginalRussianTextCopyright©2002byKh.T.Sharipov,Sh.Sh.Daminova,andL.L.TalipovaCRYSTALANDMOLECULARSTRUCTUREOFRHODIUM(III)DIISOPROPYLDITHIOPHOSPHATEKh.T.Sharipov,Sh.Sh.Daminova,andL.L.TalipovaUDC548.737Itisofinteresttodeterminethecry
2、stalstructureofthetitlecomplex,toexaminetheinteractionofrhodiumwiththeligand,andtoclarifytheroleofthedithiophosphateligandinstructureformation.Forthispurposewesynthesizedthecomplex[Rh(i-C3H7O)2PSS)3].SinglecrystalsforX-raystructureinvestigationswereobtainedbyrecrystallizationofthecomplex
3、compounds[Rh(i-C3H7O)2PSS)3]fromhotalcoholsolutionsbyheatingthesesolutionsonawaterbath.Theredprismaticcrystalsareunstableinair;topreventtheirdecay,theywerepreliminarilycoatedwithanepoxidefilm.Thecrystalsof[Rh(i-C3H7O)2PSS)3]aretriclinic.Crystaldata:a=8.7845(7),b=10.3430(8),c=18.8797(15)Å
4、,_α=81.547(2),β=88.816(2),γ=82.795(2)°,V=1683(2)Å3,M=742.70,d3,Z=2,spacegroupP1.calc=1.465g/cmThecrystallographicparametersofthesinglecrystalsweredeterminedonaBruker1KSMART/CCDdiffractometerusingamonochromatoronMoKαradiation.Forstructuralanalysiswechosesinglecrystalswithdimensions0.5×0.3
5、×0.2mmwithadsorptioncoefficientµ=1.050mm–1andF(000)=768.AfterthedatawerecorrectedforLorentzandpolarizationeffectsandweakreflectionswithI<2σ(I)(9729independentreflections)werediscarded,theworkingsetconsistedof7304reflections.Afterthefinalstageoftherefinementofthepositionalandanisotropicth
6、ermalparameters,R1=0.0527,wR2=0.0808.ThedatawereprocessedwiththeSAINTprogram[1].TheSADABSprogramwasusedtoapplyanadsorptioncorrection[2].Thestructurewassolvedbydirectmethodsandrefinedbythefull-matrixleast-squaresprocedureinanTABLE1.AtomicCoordinates(×104)andEquivalentThermalParameters(Å2×
7、103)for[Rh(i-C3H7O)2PSS)3]AtomxyzUeqAtomxyzUeqRh(1)7379(1)5571(1)7342(1)17(1)C(2)13315(4)3049(5)7661(2)52(1)S(1)7658(1)3228(1)7689(1)21(1)C(3)11601(4)1946(4)8568(2)40(1)S(2)9429(1)5015(1)6548(1)21(1)C(4)7902(3)2401(3)5940(1)25(1)S(3)9138(1)5948(1)8215(1)21(1)C(5)8482(4)26
