Crystal structures of [N(C4H9)(4)][NbCl4OAlCl3] and [N(C3H7)(4)][NbCl6]

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 P2(1)/n. (1: a =10.664(1) Angstrom, b = 14.177(1) Angstrom, c = 19.429(3) Angstrom, beta = 90.01(1)degrees, Z = 4; 2: a = 11.678(2) Angstrom, b = 15.581(2) Angstrom, c = 11.769(1) Angstrom, beta = 91.51(2)degrees, 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)degrees) with a Nb-O bond length of 1.769(4) Angstrom and a Al-O bond length of 1.771(5) Angstrom. The structure of 2 contains [N(C3H7)(4)](+) cations and [NbCl6](-)anions.