Syntheses and reactions of aluminium alkoxide compounds

Al(O(c)Hex)(3) (1) can be synthesized by the reaction of Al with cyclohexan ol under evolving of H-2 in boiling xylene. [Li{Al(OCH2Ph)(4)}] (2) was obt ained by treatment of PhCH2OH with a 1 M solution of LiAlH4 in THF. [{(THF) Li}(2){Al((OBu)-Bu-t)(4)}Cl] (3) is the result of the reaction of four equi valents of (LiOBu)-Bu-t on AlCl3 in THF. 3 is the educt for the reactions w ith the Lewis-acids InCl3 and FeCl3 in THF leading to the metalates [{(THF) (2)Li}(2){Al((OBu)-Bu-t)(4)}]. [MCl4] [M = In (4), Fe (5)]. The attempt to react InCl3 with four equivalents of LiOtBu leads to only one isolated and characterized product, the complex [Li-4((OBu)-Bu-t)(3)(THF)(3)Cl](2). THF (6.THF), which can also be synthesized by the treatment of LiCl with three equivalents of (LiOBu)-Bu-t in THF. 1-6.THF were characterized by NMR, IR a nd MS techniques as well as by X-ray structure determinations. According to them, 1, which is tetrameric in solution, is the first structurally charac terized example of the proposed trimer form of aluminium alkoxides [ROAl{Al (OR)(4)}(2)] with a central trigonal bipyramidal coordinated Al atom. 2 for ms a coordination polymer with a distorted tetrahedral coordination sphere of Li and Al, running along [100]. The trinuclear structure skeleton [{(THF )(2)Li}(2){Al((OBu)-Bu-t)(4)}](+) is still present in the isotypical metala tes 4 and 5. The counter ions [MCl4] possess nearly Td symmetry. The remark able structural motif of 6.THF are two heterocubanes [Li-4((OBu)-Bu-t)(3)(T HF)(3)Cl] dimerized by Li-Cl bonds.