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Ralf Garbe Jürgen Pebler Kurt Dehnicke Dieter Fenske Helmut Goesmann Gerhard Baum 《无机化学与普通化学杂志》1994,620(4):592-598
Phosphorane Iminato Complexes of Antimony. The Crystal Structures of [Sb2Cl5(NPMe3)2][SbCl6] · CH3CN and [SbCl(NPPh3)]2[SbCl6]2 · 6 CH3CN The title compounds are formed by reaction of antimony pentachloride in acetonitrile solution with the phosphorane iminato complexes SbCl2(NPMe3) and SbCl2(NPPh3), respectively, which themselves are synthesized by reaction of antimony trichloride with Me3SiNPR3 (R = Me, Ph). The complexionic compounds are characterized by 121Sb Mössbauer spectroscopy and by crystal structure determinations. [Sb2Cl5(NPMe3)2][SbCl6] · CH3CN: Space group P41, Z = 4, 3 698 observed unique reflections, R = 0.022. Lattice dimensions at ?60°C: a = b = 1 056.0(1), c = 2 709.6(2) pm. The structure consists of SbCl6? ions and cations [Sb2Cl5(NPMe3)2(CH3CN)]+, in which one SbIII atom and one SbV atom are bridged by the N atoms of the phosphorane iminato ligands. [SbCl(NPPh3)]2[SbCl6]2 · 6 CH3CN: Space group P1 , Z = 2, 5 958 observed unique reflections, R = 0.033. Lattice dimensions at ?60°C: a = 989.4(11), b = 1 273(1), c = 1 396(1) pm, α = 78.33(7), β = 77.27(8)°, γ = 86.62(8)°. The structure consists of SbCl6? ions and centrosymmetric cations [SbCl(NPPh3)(CH3CN)2]22+, in which the antimony atoms are bridged by the N atoms of the phosphorane iminato ligands. 相似文献