Kristallstruktur von (Ph₃PNH₂)₄[Sb₆O₁₀Cl₁₄] · 2CH₃CN / Crystal Structure of (Ph₃PNH₂)₄[Sb₆O₁₀Cl₁₄]-2CH₃CN

Abstract

Abstract The title compound has been obtained by the reaction of the phosphoraneiminato complex Cl 2 Sb(NPPh 3 ) with chlorine, followed by partial hydrolysis in acetonitrile. The colourless crystals were characterized by a crystal structure determination. Space group P1̅, Z = 2, structure refine­ment with 8320 observed unique reflections, R = 0.063 with I > 2σ(I). Lattice dimensions at -70 °C: a = 1245.0(6); b = 1277.7(8), c = 1623.8(9) pm, a = 77.97(2)°, β = 86.52(2)°, γ = 67.07(2)°. The compound consists of Ph 3 PNH 2 + ions, [Sb 6 O 10 Cl 14 ] 4- ions, in which the central unit is a Sb 4 O 6 skeleton with a double heterocubane-like arrangement with two missing corners, and of in­ cluded acetonitrile molecules without bonding interactions.