Synthesis and x-ray crystallographic characterization of (μ3-Bi)2Fe3(CO)9: A reformulation of Hieber's Bi2Fe5(CO)20 |
| |
Authors: | Melvyn Rowen Churchill James C Fettinger Kenton H Whitmire |
| |
Institution: | Department of Chemistry, State University of New York at Buffalo, Buffalo, NY 14214 U.S.A.;Department of Chemistry, Rice University, P.O. Box 1892, Houston, TX 77251 U.S.A. |
| |
Abstract: | When HFe(CO)4]? is treated first with NaBiO3 and then dilute H2SO4, a complex mixture of neutral metal carbonyl clusters results, some of which can be extracted into petroleum ether. Upon prolonged standing the extract yields a precipitate which has been characterized by X-ray crystallography as Bi2Fe3(CO)9.The complex Bi2Fe3(CO)9 crystallizes in the centrosymmetric orthorhombic space group Cmcm (D2h17; No. 63) with a 10.616(2) Å, b 13.458(3) Å, c 11.347(3) Å, V 1621.1(7) Å3 and Z = 4. Single-crystal X-ray diffraction data (Mo-Kα, 2θ = 4.5–55.0°) were collected on a Syntex P21 four-circle diffractometer and the structure was refined to RF 5.4% and RWF 4.5% for all 1039 independent data (RF 4.5% and RWF 4.5% for those 851 reflections with |F0| > 3.0σ(|F0|)). The molecule lies on a site of crystallographic C2v symmetry and is disordered. The individual molecules have a trigonal bipyramidal Bi2Fe3 core with the bismuth atoms occupying the apical sites (BiFe 2.617(2)–2.643(2) Å, FeFe 2.735(5)–2.757(5) Å). Each iron atom is linked to three terminal carbonyl ligands and the molecule has approximate C3h symmetry. The nine peripheral oxygen atoms are ordered and define a tricapped trigonal prism. The equatorial iron atoms are disordered with the two Fe3 triangles mutually displaced by approximately 30°; the disordered ensemble has approximate D3h symmetry. |
| |
Keywords: | |
本文献已被 ScienceDirect 等数据库收录! |
|