Abstract

5,11,17,23-Tetra-tert-butyl-25,27-dihydroxy-26,28-dimethoxycalix[4]arene (1, LH2) was deprotonated with two equivalents of potassium naphthalenide in THF at room temperature. The reaction of a dipotassium derivative of 1 prepared in situ with anhydrous YCl3 in a THF medium afforded the corresponding yttrium alkoxychloride [LY(thf)(μ-Cl)]2·4thf (2·4thf) in 71% yield. According to the X-ray diffraction data, complex 2 has a dimeric structure. The reaction of equimolar amounts of [(Me3Si)2N]3Y and compound 1 in a THF—toluene mixture at 60 °C was accompanied by the complete replacement of the bis(trimethylsilyl)amide ligands to form the homoligand ionic complex [LY(thf)3]+[L2Y]– (3). The structure of the latter was established by X-ray diffraction analysis.

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