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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Synthesis and structural analyses of phenylethynyl-substituted tris(2-pyridylmethyl)amines and their copper(II) complexes
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Synthesis and structural analyses of phenylethynyl-substituted tris(2-pyridylmethyl)amines and their copper(II) complexes

机译：苯乙炔基取代的三（2-吡啶基甲基）胺及其铜（II）配合物的合成与结构分析

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Three new tris(2-pyridylmethyl) amine-based ligands possessing phenylethynyl units have been prepared using Sonogashira couplings and substitution reactions. Copper(II) complexes of those tetradentate ligands have also been synthesized. Solid-state structures of the six new compounds have been determined by single-crystal X-ray diffraction analyses. Examination of the molecular structures of the ligands revealed the expected triangular geometries with virtually undeformed carbon-carbon triple bonds. While the tertiary nitrogen of the free ligands seem to be prevented from participation in supramolecular non-covalent interactions by the pyridyl hydrogen at the 3-position, the pyridyl nitrogens play a crucial role in the packing mode of the crystal structure. The nitrogens form weak hydrogen bonds, varied in length between 2.32 and 2.66 angstrom, with the pyridyl hydrogen of its neighbouring molecule. The [N center dot center dot center dot H-C] contacts enforce one-dimensional columnar assemblies on ligands that organize into wall-like structures, which in turn assemble into three-dimensional structures through CH-pi interactions. Structural analyses of Cu(II) complexes of the ligands revealed propeller-like structures caused by steric crowding of three pyridine ligands. The copper complexes of the ligands having three phenylethynyl substituents showed a remarkably deformed carbon-carbon triple bond enforced by a steric effect of the three phenyl groups. Most significantly, a total of seventy non-covalent interactions, classified into twelve types of hydrogen-involving short contacts, were identified in this study. The phenylethynyl substituent participated in forty-two interactions as a hydrogen bond acceptor, and its role was more distinctive in the crystal structures of the Cu(II) complexes.
机译：使用Sonogashira偶联和取代反应制备了三个具有苯基乙炔基单元的新的基于三（2-吡啶基甲基）胺的配体。这些四齿配体的铜（II）配合物也已经合成。六个新化合物的固态结构已通过单晶X射线衍射分析确定。对配体的分子结构的检查揭示了预期的具有几乎未变形的碳-碳三键的三角形几何形状。尽管似乎通过3-位的吡啶氢阻止了游离配体的叔氮参与超分子非共价相互作用，但吡啶氮在晶体结构的堆积方式中起着至关重要的作用。氮与周围分子的吡啶基氢形成弱的氢键，其长度在2.32至2.66埃之间变化。 [N中心点中心点中心点H-C]接触在配体上形成一维柱状组装体，这些配体组织成壁状结构，然后通过CH-pi相互作用组装成三维结构。配体的Cu（II）配合物的结构分析表明，由三个吡啶配体的空间拥挤引起的螺旋桨状结构。具有三个苯基乙炔基取代基的配体的铜配合物显示出由于三个苯基的空间效应而引起的显着变形的碳-碳三键。最重要的是，这项研究确定了总共七十种非共价相互作用，分为十二种涉及氢的短接触。苯乙炔基取代基作为氢键受体参与了42次相互作用，其作用在Cu（II）配合物的晶体结构中更具特色。

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