Institut für Anorganische Chemie, KIT, Campus Süd, Kaiserstr. 12, D-76131, Karlsruhe, Germany.
Dalton Trans. 2011 Feb 14;40(6):1365-71. doi: 10.1039/c0dt01111h. Epub 2010 Dec 22.
The chloro-bridged interpnictogen compounds [tBu₂PhSiE{BiClCH(SiMe₃)₂}₂] (E = P (4), As (5)) can be synthesized by the reaction of [tBu₂PhSiELi₂] (E = P (2), As (3)) with (Me₃Si)₂CHBiCl₂ in a molar ratio of 1 : 2. The reaction of iPr₃SiAs(SiMe₃)₂ with (Me₃Si)₂CHBiCl₂ yields the analogous compound [iPr₃SiAs{BiClCH(SiMe₃)₂}₂] (6) as well as the diarsine species [As{BiClCH(SiMe₃)₂}₂]₂ (7). Preparation of 7 is also possible in the reaction of As(SiMe₃)₃ with (Me₃Si)₂CHBiCl₂. Starting from (Me₃Si)₃SiTeSiMe₃, the Bi/Te compounds [{(Me₃Si)₃SiTe}₂BiR] (R = CH(SiMe₃)₂ (8), C(SiMe₃)₃ (9)) are obtained by the reaction with RBiCl₂ (R = CH(SiMe₃)₂, C(SiMe₃)₃ (1)). The intermediate and final products are characterized by multinuclear NMR spectroscopy and IR spectroscopy. Furthermore, crystal structures determined by X-ray diffraction are described for compounds 1 and 3-9.
氯桥联间插金属化合物 [tBu₂PhSiE{BiClCH(SiMe₃)₂}₂](E = P(4),As(5))可通过摩尔比为 1:2 的 [tBu₂PhSiELi₂](E = P(2),As(3))与(Me₃Si)₂CHBiCl₂反应合成。iPr₃SiAs(SiMe₃)₂与(Me₃Si)₂CHBiCl₂反应得到类似的化合物 [iPr₃SiAs{BiClCH(SiMe₃)₂}₂](6)和二胂物种 [As{BiClCH(SiMe₃)₂}₂]₂(7)。在 As(SiMe₃)₃与(Me₃Si)₂CHBiCl₂的反应中也可以制备 7。从(Me₃Si)₃SiTeSiMe₃出发,通过与 RBiCl₂(R = CH(SiMe₃)₂(8),C(SiMe₃)₃(9))反应,得到 Bi/Te 化合物 [{(Me₃Si)₃SiTe}₂BiR](R = CH(SiMe₃)₂(8),C(SiMe₃)₃(9))。中间体和最终产物通过多核 NMR 光谱和 IR 光谱进行表征。此外,还描述了化合物 1 和 3-9 的 X 射线衍射确定的晶体结构。