The interaction of group III metal alkyls with crown ethers. The synthesis and structure of [Ga(CH3)3]2[dibenzo18-crown-6] and [Al(CH3)3]2[dicyclohexano-18-crown-6] |
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| Institution: | 1. Bayes Business School at the University of London and CEPR, 106 Bunhill Row, London EC1Y 8TZ, United Kingdom;2. Department of Finance at Tilburg University and CEPR, 5000 LE Tilburg, the Netherlands;3. College of Finance and Statistics, Hunan University, Changsha 410082, China |
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| Abstract: | Ga(CH3)3]2dibenzo-18-crown-6] and Al(CH3)3]2dicyclohexyl-18-crown-6] were prepared by the reaction of Ga(CH3)3 or Al(CH3)3 with the appropriate crown ether in toluene. After filtering and cooling, both products were obtained as colorless, air-sensitive, rectangular crystals. The structures of both compounds were determined from single crystal X-ray diffraction data collected on a CAD-4 diffractomer. Ga(CH3)3]2dibenzo-18-crown-6] belongs to the monoclinic space group P21/c with unit cell parameters a 11.460(5), b 18.000(7), c 7.495(4) Å, β 105.65(4)°, and ?(calc) 1.32 g cm?3 for Z 2. Least-squares refinement gave a final R value of 0.061 for 1179 independent observed reflections. The molecule resides on a crystallographic center of inversion. The Ga-O distance of 2.198(8) Å is among the longest yet observed. In order to accommodate the two trialkygallium units, the crown ether is forced to adopt a chair configuration. Al(CH3)3]2dicyclohexano-18-crown-6] crystallizes in the space group P21/a with cell parameters a 16.423(7), b 9.812(5), c 20.935(8) Å, β 107.41(5)°, and ?(calc) 1.07 g cm?3 for Z 4. Least-squares refinement gave a final R value of 0.079. The flexibility of the crown ether in this case allows the bonded oxygen atoms to be positioned on the outside of the crown, with all six oxygen atoms in a near-planar arrangement. |
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