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Synthesis and Molecular Structure of [Li(THF)4][{(CO)4Mo}2(μ-PPh2)(μ-PPh2PPh2)]: The First Compound with an 1,3-Dimetalla-cyclopentaphosphane Ring [Mo(CO)4(NBD)] (NBD = norbornadiene) reacts with LiPPh2 and PPh2PPh2 in THF at –80 °C to give [Li(THF)4][{(CO)4Mo}2(μ-PPh2)(μ-PPh2PPh2)] ( 1 ). 1 exhibits an A2X coupling pattern in the 31P NMR spectrum. A crystal structure determination showed the presence of bridging phosphanido (PPh2) and diphosphane ligands (PPh2PPh2). The central Mo2P3 five-membered ring adopts a half-chair conformation and thus resembles an inorganic cyclopentane. 相似文献
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Syntheses and Crystal Structures of new Amido- und Imidobridged Cobalt Clusters: [Li(THF)2]3[Co3(μ2-NHMes)3Cl6] (1), [Li(DME)3]2[Co18(μ4-NPh)3(μ3-NPh)12Cl3] (2), [Li(DME)3]2[Co6(μ4-NPh)(μ2-NPh)6(PPh2Et)2] (3), and [Li(THF)4][Co8(μ3-NPh)6(μ2-NPh)3(PPh3)2] (4) The reactions of cobalt(II)-chloride with the lithium-amides LiNHMes and Li2NPh leads to an amido-bridged multinuclear complex [Li(THF)2]3[Co3(μ2-NHMes)3Cl6] ( 1 ) as well as to the imido-bridged cobalt cluster [Li(DME)3]2[Co18(μ4-NPh)3(μ3-NPh)12Cl3] ( 2 ). In the presence of tertiary phosphines two imido-bridged cobalt clusters [Li(DME)3]2[Co6(μ4-NPh)(μ2-NPh)6(PPh2Et)2] ( 3 ) and [Li(THF)4][Co8(μ3-NPh)6(μ2-NPh)3(PPh3)2] ( 4 ) result. The structures of 1 – 4 were characterized by X-ray single crystal structure analysis. 相似文献
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Preparation of μ-Hydrido-μ-diphenylphosphido-bis(tetracarbonylrhenium) · 1/2 Xylene and Molecular Structure of the Derivative Re2(CO)6(PPh3)2(μ-H)(μ-PPh2) (Ph = C6H5) The reaction of dirhenium decacarbonyl with diphenylphosphine in xylene solution gave at 190–200°C in a glas tube crystals of Re2(CO)8(μ-H)(μ-PPh2) · 1/2 C8H10. The obtained adduct was reacted in the same solvent with an excess of triphenylphosphine to the derivative Re2(CO)6(PPh3)2(μ-H)(μ-PPh2). Both diamagnetic dirhenium compounds with μ-H atom and μ-PPh2 group were characterized by 1H and 31P spectroscopic measurements. The molecular structure of the derivative was acertained by a single crystal X-ray analysis. Its result showed a three-membered Re2(μ-P) ring as central molecular fragment. At these Re central atoms were attached two PPh3 ligands in an unprefered cis-arrangement due to sterical reasons. A thermodynamic transinfluence of the (μ-P)? Re bond favoured the found positions of the PPh3 ligands. 相似文献
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Reactions of aqueous HX (X?Cl, Br) or of AuCl(PPh3) with Ru5(μ5-C2PPh2)(μ-PPh2)(CO)13 result in addition of the 4e-donor set (H + X) or (Au(PPh3) + Cl) with concomitant opening of two Ru? Ru bonds to give complexes containing dimetallated triangular of ‘scorpion’ cores. Aqueous HI reacts similarly, but in this case the iodide ligand spans three Ru atoms, the (H + I) set acting as 6e-donor. The structures of the two title compounds were confirmed by X-ray crystallographic studies. Ru5(μ-H)(μ5-C2PPh2)(μ-PPh2)-(μ-Br)(CO)13 is triclinic, space group P1 , a = 9.689(2), b = 11.874(2), c = 20.005(4) Å, α = 84.66(2), β = 82.90(6), λ = 67.51(6)°, Z = 2; 6478 data with I > 2σ(I) were refined to R = 0.0368, Rw = 0.0362. Ru5(μ-H)(μ5-C2PPh2)(μ3-I)(μ-PPh2)-(CO)12.CH2Cl2 is monoclinic, space group P21/n, a = 14.809(4), b = 20.721(4), c = 17.698(5) Å, β = 111.42(2)°, Z = 4; 7815 data with I > 2σ(I) were refined to R = 0.0440, Rw = 0.0416. 相似文献
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