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一种吡嗪 -2,3 -二甲酰胺配体及其硝酸银(I)配合物(一种三维配位聚合物)的晶体结构。

Crystal structure of a pyrazine-2,3-dicarboxamide ligand and of its silver(I) nitrate complex, a three-dimensional coordination polymer.

作者信息

Cati Dilovan S, Stoeckli-Evans Helen

机构信息

Debiopharm International S.A., Chemin Messidor 5-7, CP 5911, CH-1002 Lausanne, Switzerland.

Institute of Physics, University of Neuchâtel, rue Emile-Argand 11, CH-2000 Neuchâtel, Switzerland.

出版信息

Acta Crystallogr E Crystallogr Commun. 2017 May 5;73(Pt 6):798-803. doi: 10.1107/S2056989017006387. eCollection 2017 Jun 1.

Abstract

The title ligand, CHNO·2HO () [,-bis-(pyridin-4-ylmeth-yl)pyrazine-2,3-dicarboxamide], crystallized as a dihydrate. The mol-ecule is U-shaped with the carboxamide groups being to one another, making a dihedral angle of 81.6 (5)°. The terminal pyridine rings are inclined to one another by 58.5 (4)°. There is an intra-molecular N-H⋯N hydrogen bond present, forming an (5) ring motif. In the crystal, adjacent mol-ecules are linked by N-H⋯O hydrogen bonds, forming a chain along [001]. A chain of hydrogen-bonded water mol-ecules is linked to the chain of () mol-ecules by O-H⋯N hydrogen bonds, forming columns propagating along the axis. The columns are linked by C-H⋯O and C-H⋯N hydrogen bonds, forming a three-dimensional supra-molecular structure. The reaction of ligand () with silver(I) nitrate led to the formation of a new three-dimensional coordination polymer, {[Ag(CHNO)]NO} , poly[[[μ-,-bis-(pyridin-4-ylmeth-yl)pyrazine-2,3-dicarboxamide]-silver(I)] nitrate] (). The asymmetric unit is composed of half of one silver ion, located on a twofold rotation axis, half a ligand mol-ecule and half a positionally disordered nitrate anion located about a twofold rotation axis. The full mol-ecule of the ligand is generated by twofold rotational symmetry, with this twofold axis bis-ecting the C-C bonds of the pyrazine ring and the Ag-Ag bond. The carboxamide groups are now to one another, making a dihedral angle of 65.8 (4)°. The two terminal pyridine rings are inclined to one another by 6.6 (3)°. Two ligands wrap around an Ag-Ag bond of 3.1638 (11) Å, forming a figure-of-eight-shaped complex mol-ecule. Each silver ion is coordinated by two pyridine N atoms and by two carboxamide O atoms of neighbouring mol-ecules, hence forming a three-dimensional framework. The nitrate anion is linked to the framework by N-H⋯O and C-H⋯O hydrogen bonds.

摘要

标题配体CHNO·2HO()[,-双-(吡啶-4-基甲基)吡嗪-2,3-二甲酰胺]以二水合物形式结晶。分子呈U形,羧酰胺基团相互平行,二面角为81.6(5)°。末端吡啶环相互倾斜58.5(4)°。存在分子内N-H⋯N氢键,形成(5)环模式。在晶体中,相邻分子通过N-H⋯O氢键相连,沿[001]形成一条链。一条氢键连接的水分子链通过O-H⋯N氢键与()分子链相连,形成沿轴延伸的柱体。柱体通过C-H⋯O和C-H⋯N氢键相连,形成三维超分子结构。配体()与硝酸银(I)反应生成了一种新的三维配位聚合物{[Ag(CHNO)]NO} ,聚[[[μ-,-双-(吡啶-4-基甲基)吡嗪-2,3-二甲酰胺]-银(I)]硝酸盐]()。不对称单元由位于二重旋转轴上的半个银离子、半个配体分子和位于二重旋转轴周围的半个位置无序的硝酸根阴离子组成。配体的完整分子由二重旋转对称性产生,该二重轴平分吡嗪环的C-C键和Ag-Ag键。羧酰胺基团现在相互平行,二面角为65.8(4)°。两个末端吡啶环相互倾斜6.6(3)°。两个配体围绕3.1638(11)Å的Ag-Ag键缠绕,形成一个八字形复合分子。每个银离子由相邻分子的两个吡啶N原子和两个羧酰胺O原子配位,从而形成三维框架。硝酸根阴离子通过N-H⋯O和C-H⋯O氢键与框架相连。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a71/5458295/b4cd9e42da5b/e-73-00798-fig1.jpg

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