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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Stepwise formation of organometallic macrocycles and triangular prisms containing 2,2′-bisbenzimidazole ligands
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Stepwise formation of organometallic macrocycles and triangular prisms containing 2,2′-bisbenzimidazole ligands

机译：逐步形成含有2,2'-双苯并咪唑配体的有机金属大环和三角柱

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摘要

A series of organometallic macrocycles have been constructed by an efficient "bottom-up" assembly methodology at ambient temperature. Treatment of [Cp*MCl_2]_2 (1a: M = Ir, 1b: M = Rh) with pyrazine or 4,4′-bipyridine (bpy) (1:1; Cp* = pentamethylcyclopentadienyl) at room temperature resulted in the formation of binuclear complexes [Cp*MCl_2]_2(pyrazine) and [Cp*MCl_2]_2(bpy) (M = Ir or Rh), which were then further reacted with AgOTf (Tf = O_2SCF_3) and 2,2′-bisbenzimidazole ligand (BiBzIm). Four organometallic macrocyclic complexes formulated as [Cp*_4Ir_4(BiBzIm) _2(pyrazine)_2](OTf)_4 (2a), [Cp* _4Rh_4(BiBzIm)_2(pyrazine)_2](OTf) _4 (2b), [Cp*_4Ir_4(BiBzIm) _2(bpy)_2](OTf)_4 (2c) and [Cp* _4Rh_4(BiBzIm)_2(bpy)_2](OTf) _4 (2d) each bearing 2,2′-bisbenzimidazole ligand and the half-sandwich Ir, Rh fragments were finally obtained in good yields. In a similar process, if a rigid ligand L (3-pyridyl-bian) was used as the linker, two novel metallacycles (3a and 3b) which enchased a silver atom in the centre were obtained. Organometallic triangular prisms 4a were synthesized via methods similar to those of the rectangles. [Cp*IrCl_2]_2 reacted with tridentate ligand 2,4,6-tri(4-pyridyl)-1,3,5-triazine (tpt) to give the corresponding trinuclear complexes [Cp*IrCl_2] _3(tpt), then further reacted with AgOTf and 2,2′- bisbenzimidazole ligand, leading to the formation of the prism-like complexes formulated as [Cp*_6M_6(BiBzIm)_6(tpt) _2](OTf)_6 (3a: M = Ir, 3b: M = Rh). All complexes were well characterized by ~1H NMR and IR spectroscopy, as well as elemental analyses. The molecular structures of 2a, 2b, 2c, 3a, 3b and 4a were characterized by single-crystal X-ray crystallography. We found that the prism-like hexanuclear complexes 4a displayed interesting host-guest chemistry.
机译：在环境温度下，通过有效的“自下而上”组装方法已经构建了一系列有机金属大环化合物。在室温下用吡嗪或4,4'-联吡啶（bpy）（1：1; Cp * =五甲基环戊二烯基）处理[Cp * MCl_2] _2（1a：M = Ir，1b：M = Rh）导致形成双核络合物[Cp * MCl_2] _2（吡嗪）和[Cp * MCl_2] _2（bpy）（M = Ir或Rh），然后与AgOTf（Tf = O_2SCF_3）和2,2'-双苯并咪唑配体进一步反应（BiBzIm）。四种有机金属大环配合物配制成[Cp * _4Ir_4（BiBzIm）_2（吡嗪）_2]（OTf）_4（2a），[Cp * _4Rh_4（BiBzIm）_2（吡嗪）_2]（OTf）_4（2b），[Cp * _4Ir_4（BiBzIm）_2（bpy）_2]（OTf）_4（2c）和[Cp * _4Rh_4（BiBzIm）_2（bpy）_2]（OTf）_4（2d）各自带有2,2'-双苯并咪唑配体和最终以高产率获得了半夹心的Ir，Rh片段。通过类似的方法，如果使用刚性配体L（3-吡啶基-苯并）作为连接基，则获得两个在中心镶嵌了银原子的新型金属环（3a和3b）。通过类似于矩形的方法合成有机金属三角棱镜4a。 [Cp * IrCl_2] _2与三齿配体2,4,6-三（4-吡啶基）-1,3,5-三嗪（tpt）反应，得到相应的三核配合物[Cp * IrCl_2] _3（tpt），然后进一步与AgOTf和2,2'-双苯并咪唑配体反应，导致形成配制成[Cp * _6M_6（BiBzIm）_6（tpt）_2]（OTf）_6的棱柱状复合物（3a：M = Ir，3b ：M ＝ Rh）。所有配合物均通过〜1 H NMR和IR光谱以及元素分析得到了很好的表征。通过单晶X射线晶体学表征2a，2b，2c，3a，3b和4a的分子结构。我们发现，棱柱状六核配合物4a显示出有趣的宿主-客体化学。

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