Synthesis and characterization of dihydrobis(3,5-dimethylpyrazolyl)borate complexes of gallium(III) and indium(III)

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• 作者：Reger ; Daniel L. ; Pender ; Mark J. ; Caulder ; Dana L. ; Reger ; Lance. B. ; Rheingold ; Arnold L. ; et. al.
• 关键词：Gallium ; Indium ; Bis(pyrazolyl)borate
• 刊名：Journal of Organometallic Chemistry
• 出版年：1996
• 出版时间：April 19, 1996
• 年：1996
• 卷：512
• 期：1-2
• 页码：91-96
• 全文大小：456 K

文摘

The reaction of MeGaCl<sub>2sub> with one equivalent of K[H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>] yields [H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>]GaMeCl. The structure of [H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>]GaMeCl has been determined crystallographically. The molecular unit is monomeric with a distorted tetrahedral geometry around gallium. The reaction of GaCl<sub>3sub> with two equivalents of MeLi followed by one equivalent of K[H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>] yields [H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>]GaMe<sub>2sub>. Similar reactions starting with MeInCl<sub>2sub> or Me<sub>2sub>InCl yield [H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>]InMeCl and [H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>]InMe<sub>2sub>, respectively. The reaction of MeInCl<sub>2sub> with two equivalents of K[H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>] in refluxing THF yields [H<sub>2sub>B(3,5-Me<sub>2sub>pz)<sub>2sub>]<sub>2sub>InMe. In low-temperature NMR spectra of this complex (&minus;40°C), each of the three types of hydrogen atom positions shows as two sharp, equally intense resonances. Each of the pairs of resonances coalesce at higher temperatures.