N,N-Di-iso-propylcarbamato Complexes of Boron

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• 作者：Daniela Belli Dell’ ; Amico ; Fausto Calderazzo ; Luca Labella ; Fabio Marchetti
• 刊名：Inorganic Chemistry
• 出版年：2008
• 出版时间：June 16, 2008
• 年：2008
• 卷：47
• 期：12
• 页码：5372 - 5376
• 全文大小：191K
• 年卷期：v.47,no.12(June 16, 2008)
• ISSN：1520-510X

文摘

N,N-di-iso-propylcarbamato derivatives of boron(III) have been synthesized from di-iso-propylamine and boron trichloride in the presence of carbon dioxide. With a large excess of amine, a single boron product was obtained, [NH₂ⁱPr₂][B(O₂CNⁱPr₂)₄], 1, while with a lower excess a mixture of 1 and of the dinuclear derivative [B₂(O₂CNⁱPr₂)₆], 2, was produced. By heating in vacuo at 60 °C, solid 1 slowly converted to 2. The transformation was reversible, 2 giving 1 back with di-iso-propylamine under carbon dioxide at atmospheric pressure. The molecular structure of both compounds was established by X-ray diffraction methods. Compound 1 is constituted by ion-pairs where the ammonium cation is hydrogen-bonded to the mononuclear anion. Compound 2 is a dinuclear species with two bridging carbamato ligands. In both derivatives, boron shows tetrahedral coordination. As IR- and ¹H NMR spectra of the two species are well differentiated, it is possible to monitor the interconversion of 1 and 2 by both spectroscopic methods.