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- Title
Mit N-Methylpiperidin stabilisierte Halogenalane.
- Authors
Veith, Michael; Kirs, Tatjana; Huch, Volker
- Abstract
Alanes of the formula H xAl X3- x ( x = 0, 1, 2, 3; X = Cl, Br, I) and the mixed halogen species HAlClBr were synthesized as N-methyl-piperidin (nmp) adducts H xAlX3- x · znmp ( z = 1, 2) and HAlClBr ·2nmp by different routes. The crystal and molecular structures of (H3Al ·nmp)2, H2AlBr ·2nmp, H2AlI ·2nmp, the isotypic and isomorphous HAlBr2 ·2nmp, HAlI2 ·2nmp, as well as ACl3 ·nmp, ABr3 ·nmp, AI3 ·nmp, and HAlClBr ·2nmp are described. The aluminum atoms in these molecular structures either form a pentagonal bipyramid as coordination sphere with the amine bases in apical positions or are in the center of a distorted tetrahedron (AlCl3 ·nmp, ABr3 ·nmp, AI3 ·nmp). In the nmp adduct of alane, a central Al2H2 ring is formed by dimerisation of AlH3, each aluminum atom displaying a further nmp ligand together with two terminal hydrogen atoms. The influence of the halogen atoms on the hydrogen bonds in the iso-structural compounds were studied by IR spectroscopy, showing in both series H2Al X ·2nmp and HAl X2 ·2nmp ( X = Cl, Br, I) a dependence of ν(Al-H) on the substitution pattern: 1770.2-1775.2-(not measured) cm-1 (H2Al X) and 1785.0-1788.0-1791.0 cm-1 (HAl X2). The δ values of the 27Al-NMR spectra in solution show dependences on the halide numbers bonded to aluminum and display a regular growth with heavier element in the H2Al X ·2nmp series δ (27Al): 121.2 (Cl), 126.0 (Br), 131.5 (I)], whereas they have an unsteady evolution in the HAl X2 ·2nmp series [δ (27Al): 118.0 (Cl), 122.0 (Br), 108.0 (I)] and the Al X3 ·nmp series [δ (27Al): 102.1 (Cl), 104.8 (Br), 61.9 (I)].
- Publication
Zeitschrift für Anorganische und Allgemeine Chemie, 2013, Vol 639, Issue 2, p312
- ISSN
0044-2313
- Publication type
Article
- DOI
10.1002/zaac.201200459