Reinvestigation of the synthesis of phenylcalcium iodide and the first structural characterization of a heavy Grignard reagent as [((thf)2CaPhI)3 · (thf)CaO] with a central Ca4 tetrahedron |
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Authors: | Reinald Fischer Helmar Grls Matthias Westerhausen |
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Affiliation: | aInstitut für Anorganische und Analytische Chemie, Friedrich-Schiller-Universität Jena, August-Bebel-Strasse 2, D-07743 Jena, Thuringen, Germany |
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Abstract: | Phenylcalcium iodide is accessible by direct synthesis from activated calcium and iodobenzene in THF at low temperatures. The use of chloro- or bromobenzene as well as of another solvent such as diethylether lowers the yield significantly. Phenylcalcium iodide cleaves THF already at −20 °C under formation of benzene. From this reaction solution single crystals of the title compound precipitate. The central structural fragment consists of a distorted calcium tetrahedron, centered by an oxygen atom and with Ca atoms being bridged by phenyl groups (average Ca–C 257 pm) and iodide ligands. |
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Keywords: | Calcium Direct synthesis Grignard reagents Organocalcium compounds Phenylcalcium iodide |
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