Synthesis and crystal structure of a palladium dimer containing ferrocenyldiphenylphosphine, trans-[Pd(μ-Cl)(CH3)(PPh2Fc)]2

被引:0
作者
Stefanus Otto
机构
[1] Lund University,Inorganic Chemistry 1, Chemical Center
[2] University of the Free State,Department of Chemistry
来源
Journal of Chemical Crystallography | 2001年 / 31卷
关键词
palladium dimer; ferrocenyldiphenylphosphine; synthesis; crystal structure;
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摘要
The chloro-bridged dimeric complex, trans-[Pd(μ-Cl)(CH3)(PPh2Fc)]2, was prepared by reaction of [Pd(Cl)(CH3)(COD)] (COD = cis,cis-1,5-cyclooctadiene) with 1 equivalent of PPh2Fc (PPh2Fc = ferrocenyldiphenylphosphine) in acetone medium. The complex was characterized by 1H and 31P NMR spectroscopy and a single crystal X-ray diffraction study revealed a trans geometry. The compound crystallizes in the triclinic space group P1, a = 11.476(2) Å, b = 14.059(3) Å, c = 14.658(3) Å and α = 82.34(3)°, β = 75.09(3)°, and γ = 68.48(3)° with Z = 2. Most important geometrical parameters include bond lengths Pd(1)–P(1) 2.2165(10), Pd(2)–P(2) 2.2290(10), Pd(1)–C(1) 2.157(3), Pd(2)–C(2) 2.079(4), Pd(1)–Cl(1) 2.4329(13), Pd(1)–Cl(2) 2.4106(11), Pd(2)–Cl(1) 2.4169(10), and Pd(2)–Cl(2) 2.4414(13) Å and bond angles P(1)–Pd(1)–C(1) 87.47(8), P(1)–Pd(1)–Cl(2) 176.88(4), C(1)–Pd(1)–Cl(1) 173.93(7), P(2)–Pd(2)–C(2) 89.03(11), P(2)–Pd(2)–Cl(1) 174.18(4), and C(2)–Pd(2)–Cl(2) 173.50(11)°. The effective and Tolman cone angles for P(1) were calculated as 170 and 167° and that for P(2) as 179 and 177°, respectively.
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页码:185 / 190
页数:5
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