Halide‐Free Diarylcalcium Complexes—Syntheses,Structures, and Stability |
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| Authors: | Dr Jens Langer Mathias Köhler Dr Helmar Görls Prof?Dr Matthias Westerhausen |
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| Institution: | Institute of Inorganic and Analytical Chemistry, Friedrich Schiller University Jena, Humboldtstra?e 8, 07743 Jena (Germany), Fax: (+49)4?3641‐948132 |
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| Abstract: | A general procedure was developed for the synthesis of diarylcalcium complexes by addition of KOtBu to arylcalcium iodides in THF. Intermediate arylcalcium tert‐butanolate dismutates immediately leading to insoluble tert‐butanolate precipitates of calcium. Depending on the steric demand and denticity of additional neutral aliphatic azabases, mononuclear or dinuclear complexes trans‐Ca(α‐Naph)2(thf)4] ( 1 ), Ca(β‐Naph)2(thf)4] ( 2 ), Ca(Tol)2(tmeda)]2 ( 3 ), Ca(Ph)2(tmeda)]2 ( 4 ), Ca(Ph)2(pmdta)(thf)] ( 5 ), Ca(hmteta)(Ph)2] ( 6 ), and Ca(18]C‐6)(Ph)2] ( 7 ) were isolated (Naph=naphthyl; meda=N,N,N′,N′‐tetramethylethylenediamine; pmdta= N,N,N′,N′′,N′′‐pentamethyldiethylenetriamine; hmteta=N,N,N′,N′′,N′′′,N′′′‐hexamethyltriethylenetetramine). The Ca?C bond lengths vary between 250.8 and 263.5 pm, the ipso‐carbon atoms show low‐field‐shifted resonances in the 13C NMR spectra. |
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| Keywords: | calcium diarylcalcium direct synthesis N ligands Schlenk‐type equilibrium |
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