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[N(C 4 H 9 ) 4 ][NbCl 4 OAlCl 3 ]  1  crystallized after two months in form of yellow needles in a Schlenk-tube from a CH 2 Cl 2 /n-hexane solution containing equimolar amounts of [N(C 4 H 9 ) 4 ]Cl, NbCl 5  and AlCl 3 . Yellow crystals of [N(C 3 H 7 ) 4 ][NbCl 6 ]  2  yielded from the reaction of equimolar amounts of [N(C 3 H 7 ) 4 ]Cl and NbCl 5  in the same solvent. The oxygen in  1  indicates a reaction of the educts with traces of water.

Crystal structures of [N(C 4 H 9 ) 4 ][NbCl 4 OAlCl 3 ] and [N(C 3 H 7 ) 4 ][NbCl 6 ]