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  • Title: Alkyl-substituted amides as ligands in homometallic and heterobimetallic calcium complexes.
    Author: Glock C, Görls H, Westerhausen M.
    Journal: Inorg Chem; 2009 Jan 05; 48(1):394-9. PubMed ID: 19053338.
    Abstract:
    The reaction of benzylpotassium with anhydrous calcium diiodide and 2,2,6,6-tetramethylpiperidine (Tmp-H) in a molar ratio of 2:1:2 in toluene in the presence of tetramethylethylenediamine yields colorless [(tmeda)Ca(Tmp)2] (1) with an average Ca-Namide bond length of 227.5 pm. The metathesis reaction of CaI2 with 2 equiv of KN(Ph)iPr in tetrahydrofuran (THF) gives [(thf)3Ca{N(Ph)iPr}2] (2) with a Ca-N distance of 234.9 pm. An excess of KN(Ph)R (R = Me, iPr) in the metathesis reaction with CaI2 leads to the formation of calciates of the type K2Ca[N(Ph)R]4 regardless of the applied stoichiometry. The THF-free compound [K2Ca{N(Ph)Me}4]infinity (3) forms a three-dimensional net structure, whereas the amides with the larger isopropyl group lead to the formation of molecular [{(thf)2K(mu-N(Ph)iPr)2}2Ca] (4). In both of these heterobimetallic compounds, the potassium atoms bind to the pi systems of the phenyl groups. Heterobimetallic calciates [K2Ca(NPh2)4(thf)3]infinity(5) with R = Ph crystallize with a chain structure. In all of these calciates, the tetra-coordinate calcium atoms are in distorted tetrahedral environments.
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