Benzynechromium tricarbonyl. Further synthetic studies
作者： William R. Cullen , Steven J. Rettig , Hongli Zhang
DOI: 10.1016/S0020-1693(96)05252-8
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摘要: The thermolysis of Ru3(CO)11[Ph2PC6H5Cr(CO)3] affords two isomers the benzyne derivative Ru3(CO)7(C6H4) [PPhC6H5Cr(CO)3]2 ((5) and (6)). crystal structure 5, previously determined, shows phenyl groups are trans to Ru3-triangle; in 6 they probably cis on same side Ru3-triangle as moiety. Os3(CO)11[Ph6PC6H5Cr(CO)3] decomposes heating afford a less common class Os3(CO)9(C6H4)[PC6H5Cr(CO)3] (7), an electron deficient molecule Cs3(CO)8(PhPC6H4)[Ph2PC6H5Cr(CO)3] (8), which PhPC6H4 moiety acts four-electron donor. isopropylphosphine derivatives M3(CO)11[Pri2PC6H5Cr(CO)3] (M=Ru, Os), also, undergo HRu3(CO)8[C6H4Cr(CO)3](PPri2) (10), Ru(CO)3[Pri2PC6H5Cr(CO)3]2 (11), H2Os3(CO)8[PriPC6H4Cr(CO)3]) (12) H2Os3(CO)8[PriPC6H4Cr(CO)3](Pri2PC6H5-Cr(CO)3] (13). Complex 10 is benzynechromium tricarbonyl with CrRu bond. phosphines complex 11, Ru(CO)5. structures complexes 12 13 closely related orthometalated [PC6H4Cr(CO) 3] acting donor cluster. Crystal data: for 8 (C41H24CrO11Os3P2·CH2Cl2): monoclinic, ; 11 (C33H38Cr2O9P2Ru): (C21H13CrO12Os3P): orthorhombic, (C35H32Cr2O14Os3P2·2CH2Cl2): . were solved by Patterson methods refined full-matrix least-squares procedures R = 0.057, 0.031, 0.030 0.032 (Rw 0.065, 0.030, 0.028 0.030) 6320, 6103, 3529 6042 reflections I≥3σ(I), respectively.
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