A structural study of bis-(trimethylamine)alane, AlH<inf>3</inf>·2NMe<inf>3</inf>, by variable temperature X-ray crystallography and DFT calculations
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The structure of AlH3·2NMe3 has been investigated by single-crystal X-ray diffraction over the range of 296-173 K. Over this temperature range a phase change is observed from Cmca to Pbcm where the methyl groups convert from a statistically disordered conformation to adopt a mutually eclipsed conformation at lower temperatures. Measurement of the unit cell dimensions shows a decrease in the lengths of the a and b axes, and an increase in that of the c axis as the temperature is lowered, with inflections apparent between 223 and 233 K in the region of the phase change. Low-temperature DSC measurements reveal the change from Pbcm to Cmca to occur at 218.3 K, with an enthalpy of 107.7 J mol-1. The molecular structure of AlH3·2NMe3 is compared with those of related amine adducts of Group 13 hydrides, either measured experimentally or calculated using DFT methods. 1H, 13C and 27Al NMR spectroscopy has also been utilized to characterize AlH3·2NMe3 and its 1:1 counterpart AlH3·NMe3. © 2009 Elsevier B.V. All rights reserved.
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