Crystal and molecular structures of Os3(CO)9[μ3-(C5H4PR)Fe(C5H4)] (R Fc or Ph), two molecules with Fe → Os bonds
作者： William R. Cullen , Steven J. Rettig , Cai Zheng Tu
DOI: 10.1016/0022-328X(93)83178-X
关键词: Octane 、 Metallocene 、 Yield (chemistry) 、 Stereochemistry 、 Chemistry 、 Cyclophane 、 Moiety 、 Triclinic crystal system 、 Crystallography 、 Ring (chemistry) 、 Molecule
摘要: Abstract The thermal reaction between OS3(CO)12 and Fe(C5H4)2PPh affords Os3(CO)9[μ3-(C5H4PPh)Fe(C5H4)] (5b) (70%) as the only major product. Heating a solution of Os3(CO)11(PFc2Ph) (FcH (η-C5H5)2Fe) in octane for 3 h gives related molecule Os3(CO)9[μ3-(C5H4PFc)Fe(C5H4)] (5a) low yield (5%). structures 5a 5b have been established by X-ray crystallography, revealing each case that closed Os3-triangle is capped on one face ferrocenyl phosphido moiety acting an overall six-electron donor. It bonded to cluster via phosphorus atom, carbon atom from C5H4 ring, iron atom. Two semibridging carbonyls are also present structure. Crystals (μ3-[η5-C5H4)2 Fe]P[(η5-C5H4)Fe(η5,C5H5)]-Fe,P,P,COs3(CO)9 triclinic, 12.304(1),b 12.336(2), c 10.886(2) A, α 115.38(2), β 92.34(1), γ 91.76(1)°, Z 2, space group P 1 , those {μ3-η4-[(η5-C5H4)2Fe]P(C6H5)]-Fe,P,P,C Os3(CO)9·O.5CH2Cl2 12.427(2), b 13.061(1), 9.209(1) 96.562(8), 91.25(1), 76.956(9)°, 2, . were solved heavy methods refined full-matrix least-squares procedures R 0.036 0.031 5884 4716 reflections with I ⩾ 3σ (I), respectively.
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