Synthesis, crystal structure, and reactivity of a four-coordinate iron(II) chloride complex bearing the sterically demanding tert-butyl-tris(3-isopropylpyrazolyl)borato ligand |
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Authors: | Olivier Graziani Mats Tilset |
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Affiliation: | a UMR 6226 “Sciences Chimiques de Rennes”, CNRS, Université de Rennes 1, Campus de Beaulieu, F-35042 Rennes Cedex, France b UMR 6626 CNRS, Université de Rennes 1, Groupe Matière Condensée et Matériaux, Campus de Beaulieu, F-35042 Rennes Cedex, France c Department of Chemistry, University of Oslo, P.O. Box 1033, Blindern, N-0315 Oslo, Norway |
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Abstract: | The salt elimination reaction between FeCl2(THF)1.5 and the sterically hindered thallium tert-butyl-tris(3-isopropylpyrazolyl)borate, Tl[t-BuTpi-Pr], affords the new air and moisture-sensitive, high-spin, four-coordinate complex Fe[t-BuTpi-Pr]Cl (1) in 52% yield. Compound 1 has been characterized by elemental analysis, paramagnetic 1H NMR, and X-ray crystal structure determination. Fe[t-BuTpi-Pr]Cl is monomeric, and the homoscorpionate ligand is κ3-coordinated. The Fe(II) ion lies in a trigonally distorted tetrahedral environment with average N-Fe-N and N-Fe-Cl angles of 89.4(2)° and 125.7(2)°, respectively. Upon reactions with methyllithium followed by carbonylation, the six-coordinate acetyl-dicarbonyl derivative Fe[t-BuTpi-Pr](CO)2{C( O)Me} was identified by IR spectroscopy. The reaction of 1 with ethylmagnesiumbromide furnished a mixture of mononuclear Grignard complexes Mg[t-BuTpi-Pr]X (X = Et, Cl, Br), resulting formally from a facile and quantitative replacement of the [Fe-Cl]+ fragment by [Mg-X]+. |
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Keywords: | Iron complex N-ligand Tris(pyrazolyl)borate Crystal structure Four-coordinate complex |
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