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>CO replacement in Ru3(CO)12by 2,3-bis(diphenylphosphino)maleic anhydride (bma). X-ray structures of Ru3(CO)10(bma)·H2O and
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CO replacement in Ru3(CO)12by 2,3-bis(diphenylphosphino)maleic anhydride (bma). X-ray structures of Ru3(CO)10(bma)·H2O and
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机译:CO replacement in Ru3(CO)12by 2,3-bis(diphenylphosphino)maleic anhydride (bma). X-ray structures of Ru3(CO)10(bma)·H2O and
Thermolysis of Ru3(CO)12with 2,3-bis(diphenylphosphino)maleic anhydride (bma) in toluene solution gives the new compounds Ru3(CO)10(bma) (2), Ru2(CO)6(bma) (3), and(4). All compounds have been isolated and characterized in solution by IR and31P NMR spectroscopy. The solid-state structures of2, as the monohydrate, and4were established by X-ray crystallography. Ru3(CO)10(bma)·H2O crystallizes in the monoclinic space groupC2/c,a=12.741(2) Å,b=19.548(2) Å,c=32.973(4) Å, β=96.847(9)°,V=8154(2) Å3,Z=8,dcalc=1.740 g cm−3;R=0.046,Rw=0.051 for 2541 observed reflections withl>3σ(l). The bma ligand in2is bound to the triruthenium frame in a bridging fashion, with equatorially disposed PPh2groups. The X-ray structure of2reveals an extreme twisting of the maleic anhydride ring away from the plane defined by the plane of the three ruthenium atoms, along with a significant lengthening of the maleic anhydride C=C π bond.crystallizes in the monoclinic space groupP21/c,a=9.3113(5) Å,b=18.164(1) Å,c=20.097(1) Å, β-102.021(4)°,V=3324.5(3) Å3,Z=4,dcalc=1.671 g cm−3;R=0.024,Rw=0.030 for 3499 observed reflections withl>3σ(l). The presence of the μ2moiety and P−C (maleic anhydride) bond cleavage attendant in the formation of4are confirmed by X-ray analysis. The relationship of the compounds3and4to the dimeric compounds Ru2(CO)6(bpcd) andwhere bpcd=4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione is discussed. Independent studies dealing with Ru3(CO)10(bma) (bridging isomer) have shown that cluster2is stable in toluene solution at elevated temperature and does not afford compounds3and4, suggesting the intermediacy of the putative chelating isomer of Ru3(CO)10(bma) (1)
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