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X-ray structural characterization of [Et4N+]3[BiFe4(CO)163−]

1986; Elsevier BV; Volume: 303; Issue: 1 Linguagem: Inglês

10.1016/0022-328x(86)80115-2

1872-8561

Melvyn Rowen Churchill, James C. Fettinger, Kenton H. Whitmire, Craig B. Lagrone,

Synthesis and characterization of novel inorganic/organometallic compounds

Sodium bismuthate has previously been reported to react with Fe(CO)5 in methanolic KOH, producing the [BiFe4(CO)163−] anion. [Et4N+]3[BiFe4(CO)163−] crystallizes in the centrosymmetric monoclinic space group P21/n with a 13.497(2), b 19.765(3), c 19.275(3) Å, β 91.086(13)°, V 5141.0(15) Å3, Z = 4. Diffraction data (2θ = 4.5–45.0°, using Mo-Kα radiation) were collected with a Syntex P21 automated four-circle diffractometer and the structure was refined to RF 7.5% and RwF 6.1% for those 4306 reflections with |Fo| > 3σ(|Fo|). The [BiFe4(CO)163−] anion contains a central bismuth tetrahedrally surrounded by Fe(CO)4 units, with an average Bi—Fe distance of 2.750(2) Å. Each iron atom is in a trigonal-bipyramidal environment. The three Et4N+ cations are all disordered.