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THE INTERACTION OF GROUP III METAL ALKYLS WITH CROWN ETHERS. THE SYNTHESIS AND STRUCTURE OF 2 AND 2
2 and 2 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 diffractometer. 2 belongs to the monoclinic space group P21/c with unit cell parameters a 11.460(5), b 18.000(7), c 7.495(4) Angstroem, beta 105.65(4) degree, and rho(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) Angstroem is among the longest yet observed.In order to accomodate the two trialkylgallium units, the crown ether is forced to adopt a chair configuration. 2 crystallizes in the space group P21/a with cell parameters a 16.423(7), b 9.812(5), c 20.935(8) Angstroem, beta 107.41(5) degree, and rho(calc) 1.07 g cm-3 for Z = 4.Least-squares refinement gave a final R value of 0.079.The greater 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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Reference£º
Chiral Catalysts,
Chiral catalysts – SlideShare