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Abstract
The organoaluminum complex [Al(CH3)]2[15]aneN4[Al(CH3)3]2 was prepared by reaction of an excess of trimethylaluminum with the macrocyclic tetradentate secondary amine [15]aneN4 in toluene. Isolated as large, colourless, extremely air-sensitive, prismatic crystals, [Al(CH3)]2[15]aneN4[Al(CH3)3]2 was characterized by single crystal X-ray diffraction: the title compound crystallizes in the monoclinic space group P21/n with unit cell parameters a = 10.826(2)Å, b = 18.221(5) Å, c = 13.825(4)Å, β = 102.23(2)°, V = 2665.3Å3 and D c = 1.09gcm−3 for Z = 4. Least-squares refinement based on 2064 observed reflections converged at R = 0.056, R w = 0.065. The distortion displayed by the macrocycle is quite extensive. A planar four-membered Al2N2 ring occupies the central cavity of the macrocycle. The mean Al[sbnd]N distance in the Al2N2 fragment is 1.958(5)Å while the mean Al[sbnd]N[sbnd]Al angle is 90.6(2)°. The Al … Al contact is 2.785(3)Å.