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首页> 外文期刊>Acta crystallographica. Section C, Structural chemistry. >Mono- and binuclear tris(3-tert-butyl-2-sulfanyl-idene-1 H-imidazol-1 -yl)hydroborate bismuth(lll) dichloride complexes: a soft scorpionate ligand can coordinate to p-block elements
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Mono- and binuclear tris(3-tert-butyl-2-sulfanyl-idene-1 H-imidazol-1 -yl)hydroborate bismuth(lll) dichloride complexes: a soft scorpionate ligand can coordinate to p-block elements

机译：单颗核三（3-叔丁基-2-磺酰基 - 伊胺-1H-咪唑-1-基）水硼酸铋（LLL）二氯化物配合物：柔软的蝎子配体可以与P嵌段元件协调

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摘要

Tris(pyrazolyl)hydroborate ligands have been utilized in the fields of inorganic and coordination chemistry due to the ease of introduction of steric and electronic substitutions at the pyrazole rings. The development and use of the tris(pyrazolyl)hydroborate ligand, called a 'scorpionate', were pioneered by the late Professor Swiatoslaw Trofimenko. He developed a second generation for his ligand system by the introduction of 3-tert-butyl and 3-phenyl substituents and this new ligand system accounted for many remarkable developments in inorganic and coordination chemistry in stabilizing monomeric species while maintaining an open coordination site. Bismuth is remarkably harmless among the toxic heavy metal p-block elements and is now becoming popular as a replacement for highly toxic metal elements, such as lead. Two bismuth(III) complexes of the anionic sulfur-containing tripod tris(3-tert-butyl-2-sulfanyl-idene-1H-imidazol-l-yl)hydroborate ligand were prepared. By recrystallization from MeOH/CH_2Cl_2, orange crystals of dichlorido(methanol-κO)[tris(3-tert-butyl-2-sulfanylidene-1H-imidazol-1-yl-κS')hydroborato]bismuth(III), [Bi(C_21-H_34BN__6S_3)Cl_2(CH_4O)], (I), were obtained, manifesting a mononuclear structure. By using a noncoordinating solvent, red crystals of the binuclear structure with bridging Cl atoms were obtained, namely di-μ-chlorido-bis{chlorido[tris(3-tert-butyl-2-sulfanylidene-l.￡Wmidazol-l-yl-κS)hydroborato]bismuth(III)}, [Bi_2-(C_21H_34BN_6S_3)_2Cl_4], (II). These complexes show {Bi~IIIS_3Cl_2O} and {Bi~IIIS_3Cl_3} coordination geometries with average Bi~III—S bond lengths of 2.73 and 2.78 A in (I) and (II), respectively. The overall Bi~III coordination geometry is distorted octahedral due to stereochemically active lone pairs. The three Bi~III—S bond lengths are almost equal in (I) but show considerable differences in (II), with one long and two shorter distances that also correlate with changes in the UV-Vis and ~1H NMR spectra. For direct measurements of the Bi—S/Cl coordination, ligand K-edge X-ray absorption measurements were carried out in combination with ground and excited-state electronic structure analyses. For p-block elements, these sulfur-containing ligands are useful for preparing the appropriate complexes due to their flexible coordination geometry.
机译：由于吡唑环的易于引入空间和电子取代的易于引入，已经在无机和协调化学领域使用了TRIS（吡唑基）氢硼酸盐配体。 Tris（吡唑基）水硼酸盐配体的开发和使用称为“蝎子”，由Swiatoslaw Trofimenko的后期教授开创。他通过引入3-叔丁基和3-苯基取代基来开发了他的配体系统的第二代，并且这种新配体系统占无机和配位化学的许多显着发展，同时保持开放的配位部位。铋在有毒重金属P嵌段元件中具有显着无害，并且现在变得流行为诸如铅的高毒性金属元素的替代品。制备了两种含阴离子硫的三架三架Tris（3-叔丁基-2-磺酰基 - 偶胺-1H-咪唑-1-炔胺-1H-咪唑-1-基）水合配体的两种铋（III）络合物。通过从MeOH / CH_2Cl_2中重结晶，二氯二甲醚（甲醇-2-巯基-1H-咪唑-1-基-1-κB）的橙色晶体（III），[BI（获得C_21-H_34BN__6S_3）CL_2（CH_4O）]，（I），表现出单核结构。通过使用非环化溶剂，获得具有桥接Cl原子的双核结构的红色晶体，即Di-μ-氯 - BIS（氯）[Tris（3-叔丁基-2-巯基-1。£Wmidazol-L-Y1 -κS）氢硼丙酸盐]铋（III）}，[Bi_2-（C_21H_34BN_6S_3）_2CL_4]，（II）。这些复合物在（i）和（ii）中，平均Bi〜IIIS_3CL_2O}和{Bi〜IIIS_3CL_2O}和{BI〜IIIS_3CL_3}和{BI〜IIIS_3CL_3}的平均BI〜III-S键合长度分别为2.73和2.78A。由于立体化学活性孤立对，总体BI〜III协调几何形状被扭曲的八面体。三个Bi〜III-S键长度在（i）中几乎相等，但在（ii）中显示了相当大的差异，其中一个长而两个较短的距离，也与UV-Vis和〜1H NMR光谱的变化相关。对于Bi-S / Cl的直接测量，与地面和激发状态电子结构分析结合进行配体k边缘X射线吸收测量。对于P嵌段元件，这些含硫配体可用于制备由于其柔性配位几何形状而制备适当的络合物。

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