Abstract
[N(C4H9)4][NbCl4OAlCl3] 1 crystallized after two months in form of yellow needles in a Schlenk-tube from a CH2Cl2/n-hexane solution containing equimolar amounts of [N(C4H9)4]Cl, NbCl5 and AlCl3. Yellow crystals of [N(C3H7)4][NbCl6] 2 yielded from the reaction of equimolar amounts of [N(C3H7)4]Cl and NbCl5 in the same solvent. The oxygen in 1 indicates a reaction of the educts with traces of water. Both compounds crystallize in the space group P21/n. (1: a=10.664(1)Å, b=14.177(1)Å, c=19.429(3)Å, β=90.01(1)°, Z=4; 2: a=11.678(2)Å, b=15.581(2)Å, c=11.769(1)Å, β=91.51(2)°, Z=4). 1 is characterized by [N(C4H9)4]+ cations and [NbCl4OAlCl3] units which are linked by chlorine bridges to dimeric anions. [NbCl4OAlCl3]- has a nearly linear Nb-O-Al bridge (bond angles 178.9(3)°) with a Nb-O bond length of 1.769(4) Å and a Al-O bond length of 1.771(5) Å. The structure of 2 contains [N(C3H7)4]+ cations and [NbCl6]- anions.
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