New tertiary phosphine derivatives of Os3(CO)12: X-ray structures of 1,2-[Os3(CO)10{PhP(o-Tol)2}2], 1,2,3-[Os3(CO)9{(4-FC6H4)3P}3], 1,2,3-[Os3(CO)9{PhP(Cy)2}3] and [Os3(μ-OH)2(CO)8{(4-FC6H4)3P}2]

摘要

Reactions of 1,2-[Os3(CO)10(NCMe)2](1) with tertiary phosphines such astris(4-fluorophenyl)phosphine(4-FC6H4)3P, bis(o-tolyl)(phenyl)phosphine PhP(o-Tol)2and dicyclohexyl(phenyl)phosphine PhP(Cy)2 have been examined atroom temperature and found to yield the di- and tri-substituted products 1,2-[Os3(CO)10(PR3)2]{(2), PR3 = (4-FC6H4)3P;(3), PR3 = PhP(o-Tol)2;(4), PR3 = PhP(Cy)2} and 1,2,3-[Os3(CO)9(PR3)3] {(5), PR3 = (4-FC6H4)3P;(6), PR3 = PhP(o-Tol)2;7, PR3 = PhP(Cy)2}as the major products, in addition to the dihydroxyl-bridged complexes 1,2-[Os3(CO)8(PR3)2(μ-OH)2]{(8), PR3 = (4-FC6H4)3P;(9), PR3 = PhP(o-Tol)2;(10), PR3 = PhP(Cy)2} in trace amounts. Compounds (2)-(10) have been characterized by a combination of elemental analyses,infrared, NMR and mass spectral data together with single crystal X-ray diffraction studies for (3), (5), (7) and (8).