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聚[[μ-氯-μ-(2,3-二甲基吡嗪)-铜(I)]乙醇半溶剂合物]的合成与晶体结构,其展现出一种新的异构CuCl(2,3-二甲基吡嗪)网络。

Synthesis and crystal structure of poly[[μ-chlorido-μ-(2,3-di-methyl-pyrazine)-copper(I)] ethanol hemisolvate], which shows a new isomeric CuCl(2,3-di-methyl-pyrazine) network.

作者信息

Näther Christian, Jess Inke

机构信息

Institut für Anorganische Chemie, Universität Kiel, Max-Eyth.-Str. 2, 24118 Kiel, Germany.

出版信息

Acta Crystallogr E Crystallogr Commun. 2024 Sep 24;80(Pt 10):1059-1063. doi: 10.1107/S2056989024009174. eCollection 2024 Sep 1.

DOI:10.1107/S2056989024009174
PMID:39372189
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11451487/
Abstract

Reaction of copper(I)chloride with 2,3-di-methyl-pyrazine in ethanol leads to the formation of the title compound, poly[[μ-chlorido-μ-(2,3-di-methyl-pyrazine)-copper(I)] ethanol hemisolvate], {[CuCl(CHN)]·0.5CHOH} or CuCl(2,3-di-methyl-pyrazine) ethanol hemisolvate. Its asymmetric unit consists of two crystallographically independent copper cations, two chloride anions and two 2,3-di-methyl-pyrazine ligands as well as one ethanol solvate mol-ecule in general positions. The ethanol mol-ecule is disordered and was refined using a split model. The methyl H atoms of the 2,3-di-methyl-pyrazine ligands are also disordered and were refined in two orientations rotated by 60° relative to each other. In the crystal structure, each copper cation is tetra-hedrally coordinated by two N atoms of two bridging 2,3-di-methyl-pyrazine ligands and two μ-1,1-bridg-ing chloride anions. Each of the two copper cations are linked by pairs of bridging chloride anions into dinuclear units that are further linked into layers bridging 2,3-di-methyl-pyrazine coligands. These layers are stacked in such a way that channels are formed in which the disordered solvent mol-ecules are located. The topology of this network is completely different from that observed in the two polymorphic modifications of CuCl(2,3-di-methyl-pyrazine) reported in the literature [Jess & Näther (2006). , 7446-7454]. Powder X-ray diffraction measurements reveal that the title compound is unstable and transforms immediately into an unknown crystalline phase.

摘要

氯化亚铜与2,3-二甲基吡嗪在乙醇中反应生成标题化合物聚[[μ-氯代-μ-(2,3-二甲基吡嗪)-铜(I)]乙醇半溶剂化物],{[CuCl(C₄H₆N₂)]·0.5C₂H₅OH}或CuCl(2,3-二甲基吡嗪)乙醇半溶剂化物。其不对称单元通常包含两个晶体学独立的铜阳离子、两个氯离子阴离子、两个2,3-二甲基吡嗪配体以及一个乙醇溶剂分子。乙醇分子无序,采用分裂模型进行精修。2,3-二甲基吡嗪配体的甲基氢原子也无序,以相对于彼此旋转60°的两个取向进行精修。在晶体结构中,每个铜阳离子由两个桥连的2,3-二甲基吡嗪配体的两个氮原子和两个μ-1,1-桥连的氯离子阴离子进行四面体配位。两个铜阳离子中的每一个都通过成对的桥连氯离子阴离子连接成双核单元,这些双核单元进一步连接成桥连2,3-二甲基吡嗪共配体的层。这些层以形成通道的方式堆叠,无序的溶剂分子位于通道中。该网络的拓扑结构与文献中报道的CuCl(2,3-二甲基吡嗪)的两种多晶型变体中观察到的拓扑结构完全不同[Jess & Näther (2006). , 7446 - 7454]。粉末X射线衍射测量表明,标题化合物不稳定,会立即转变为未知的晶相。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/d8cd0248035f/e-80-01059-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/65262faefbf5/e-80-01059-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/666a32be8331/e-80-01059-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/375b3fe9c776/e-80-01059-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/d8cd0248035f/e-80-01059-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/65262faefbf5/e-80-01059-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/666a32be8331/e-80-01059-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/375b3fe9c776/e-80-01059-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ea2d/11451487/d8cd0248035f/e-80-01059-fig4.jpg

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