Structural characterization of Al10O6iBu16(μ-H)2, a high aluminum content cluster: Further studies of methylaluminoxane (MAO) and related aluminum complexes
The first structurally characterized isobutyl-containing aluminoxane compound is presented. The Al10O6iBu 16(μ-H)2 (I) cluster is produced from neat octakis-isobutyltetraluminoxane (Al4O2iBu 8) at 80°C in 6-8 h followed by slow crystallization. The crystal is triclinic (space group P1) with the molecule lying on an inversion center. This aluminoxane contains both nearly linear, 154(2)°, aluminum-bridging hydrides and three-coordinate aluminum sites. Solid-state 27Al magic-angle spinning (MAS) NMR experiments were done at 19.6 and 40 T (833 MHz and 1.703 GHz, 1H) and at 30-35 kHz spinning speeds, leading to the determination of the Cq and η values for the two four-coordinate Al sites and a lower limit of Cq for the three-coordinate Al site. Geometry-optimized restricted Hartree-Fock calculations at the double-ζ level of an idealized structure (methyl substituted, D2h geometry) yielded Cq and η in close agreement with experiment; C q agrees within 3 MHz. © 2007 American Chemical Society.
Publication Source (Journal or Book title)
Wu, F., Simeral, L., Mrse, A., Eilertsen, J., Negureanu, L., Gan, Z., Fronczek, F., Hall, R., & Butler, L. (2007). Structural characterization of Al10O6iBu16(μ-H)2, a high aluminum content cluster: Further studies of methylaluminoxane (MAO) and related aluminum complexes. Inorganic Chemistry, 46 (1), 44-47. https://doi.org/10.1021/ic060291y