ISSN:
0947-6539
Keywords:
aluminium
;
gallium
;
hydrolyses
;
Si ligands
;
structure elucidation
;
Chemistry
;
General Chemistry
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Notes:
The reactions of [(Me3Si)3CLi2thf] with Me2MCl (M = Al, Ga) afford the mixed trialkylmetallanes [(Me3Si)3-CAlMe2·thf] (1) and [(Me3Si)3 CGaMe2·thf] (2) in high yields. The coordinated THF molecule of compound 2 can be removed by sublimation in vacuo to yield the solvent-free product [(Me3Si)3-CGaMe2] (3). Hydrolysis of compound 2 with one equivalent of water at 0°C gives the trimeric hydroxide [{(Me3Si)3CGaMe(μ-OH)}3] (4), while the reaction with two equivalents of water at room temperature yields the unusually stable gallium hydroxide-water complex [{(Me3Si)3CGaMe(OH)(μ-OH)MeGaC(SiMe3)3) H2O·2thf] (6). On heating, compound 6 is converted to the hydroxide [{(Me3Si)3C}4Ga4(μ-O)2(μ -OH)4] (5), which has a heteroadamantane-like core. The hydrolysis of compound 1 with one equivalent of water at - 25°C gives the dimeric hydroxide [{(Me3Si)3CAlMe(μ-OH)}2·2thf] (7), while the reaction with two equivalents of water results in the formation of the novel hydroxide [{(Me3Si)3C}4Al4(μ-O)2 (μ-OH)4] (8), which is isostructural to the gallium compound 6 with the adamantane-like structure. The molecular structures of compounds 1, 2, 4, 5·3THF, 6, 7 and 8·0.5 THF have been determined by X-ray structure analysis. Compound 7 is the first structurally characterised aluminium hydroxide containing methyl groups, and 8 is the smallest structurally characterised galloxane hydroxide described in literature.
Additional Material:
7 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/chem.19970031109
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