{"title":"聚[[μ-氯-μ-(2,3-二甲基吡嗪)-铜(I)]乙醇半异醇酸酯]的合成与晶体结构,它显示了一种新的异构 CuCl(2,3-二甲基吡嗪)网络。","authors":"Christian Näther , Inke Jess","doi":"10.1107/S2056989024009174","DOIUrl":null,"url":null,"abstract":"<div><div>In the crystal structure of the title compound, the copper cations are each tetrahedrally coordinated by two 2–3-dimethylpyrazine ligands and two chloride anions and linked into dinuclear units that are further connected into layers by bridging 2,3-dimethylpyrazine ligands.</div></div><div><div>Reaction of copper(I)chloride with 2,3-dimethylpyrazine in ethanol leads to the formation of the title compound, poly[[μ-chlorido-μ-(2,3-dimethylpyrazine)-copper(I)] ethanol hemisolvate], {[CuCl(C<sub>6</sub>H<sub>8</sub>N<sub>2</sub>)]·0.5C<sub>2</sub>H<sub>5</sub>OH}<sub>n</sub> or CuCl(2,3-dimethylpyrazine) ethanol hemisolvate. Its asymmetric unit consists of two crystallographically independent copper cations, two chloride anions and two 2,3-dimethylpyrazine ligands as well as one ethanol solvate molecule in general positions. The ethanol molecule is disordered and was refined using a split model. The methyl H atoms of the 2,3-dimethylpyrazine 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 tetrahedrally coordinated by two N atoms of two bridging 2,3-dimethylpyrazine ligands and two μ-1,1-bridging 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 <em>via</em> bridging 2,3-dimethylpyrazine coligands. These layers are stacked in such a way that channels are formed in which the disordered solvent molecules are located. The topology of this network is completely different from that observed in the two polymorphic modifications of CuCl(2,3-dimethylpyrazine) reported in the literature [Jess & Näther (2006). <em>Inorg. Chem.</em><strong>45</strong>, 7446–7454]. Powder X-ray diffraction measurements reveal that the title compound is unstable and transforms immediately into an unknown crystalline phase.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 10","pages":"Pages 1059-1063"},"PeriodicalIF":0.5000,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451487/pdf/","citationCount":"0","resultStr":"{\"title\":\"Synthesis and crystal structure of poly[[μ-chlorido-μ-(2,3-dimethylpyrazine)-copper(I)] ethanol hemisolvate], which shows a new isomeric CuCl(2,3-dimethylpyrazine) network\",\"authors\":\"Christian Näther , Inke Jess\",\"doi\":\"10.1107/S2056989024009174\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>In the crystal structure of the title compound, the copper cations are each tetrahedrally coordinated by two 2–3-dimethylpyrazine ligands and two chloride anions and linked into dinuclear units that are further connected into layers by bridging 2,3-dimethylpyrazine ligands.</div></div><div><div>Reaction of copper(I)chloride with 2,3-dimethylpyrazine in ethanol leads to the formation of the title compound, poly[[μ-chlorido-μ-(2,3-dimethylpyrazine)-copper(I)] ethanol hemisolvate], {[CuCl(C<sub>6</sub>H<sub>8</sub>N<sub>2</sub>)]·0.5C<sub>2</sub>H<sub>5</sub>OH}<sub>n</sub> or CuCl(2,3-dimethylpyrazine) ethanol hemisolvate. Its asymmetric unit consists of two crystallographically independent copper cations, two chloride anions and two 2,3-dimethylpyrazine ligands as well as one ethanol solvate molecule in general positions. The ethanol molecule is disordered and was refined using a split model. The methyl H atoms of the 2,3-dimethylpyrazine 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 tetrahedrally coordinated by two N atoms of two bridging 2,3-dimethylpyrazine ligands and two μ-1,1-bridging 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 <em>via</em> bridging 2,3-dimethylpyrazine coligands. These layers are stacked in such a way that channels are formed in which the disordered solvent molecules are located. The topology of this network is completely different from that observed in the two polymorphic modifications of CuCl(2,3-dimethylpyrazine) reported in the literature [Jess & Näther (2006). <em>Inorg. Chem.</em><strong>45</strong>, 7446–7454]. Powder X-ray diffraction measurements reveal that the title compound is unstable and transforms immediately into an unknown crystalline phase.</div></div>\",\"PeriodicalId\":7367,\"journal\":{\"name\":\"Acta Crystallographica Section E: Crystallographic Communications\",\"volume\":\"80 10\",\"pages\":\"Pages 1059-1063\"},\"PeriodicalIF\":0.5000,\"publicationDate\":\"2024-09-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451487/pdf/\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Acta Crystallographica Section E: Crystallographic Communications\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://www.sciencedirect.com/org/science/article/pii/S205698902400207X\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CRYSTALLOGRAPHY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Acta Crystallographica Section E: Crystallographic Communications","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/org/science/article/pii/S205698902400207X","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CRYSTALLOGRAPHY","Score":null,"Total":0}
引用次数: 0
摘要
氯化铜(I)与 2,3-二甲基吡嗪在乙醇中反应生成了标题化合物,即聚[[μ-氯-μ-(2,3-二甲基吡嗪)-铜(I)]乙醇半溶液酸盐],{[CuCl(C6H8N2)]-0.5C2H5OH} n 或 CuCl(2,3-二甲基吡嗪)乙醇半溶液酸盐。它的不对称单元由两个晶体学上独立的铜阳离子、两个氯阴离子、两个 2,3-二甲基吡嗪配体以及一个一般位置的乙醇溶解分子单元组成。乙醇分子单元是无序的,采用分裂模型进行了细化。2,3-二甲基吡嗪配体的甲基 H 原子也是无序的,并以两个相对旋转 60° 的方向进行了细化。在晶体结构中,每个铜阳离子都由两个桥接的 2,3-二甲基吡嗪配体的两个 N 原子和两个μ-1,1-桥接的氯阴离子四面体配位。每两个铜阳离子通过成对的桥接氯阴离子连接成双核单元,再通过桥接 2,3-二甲基吡嗪配体连接成层。这些层的堆叠方式形成了通道,而无序的溶剂分子则位于通道中。该网络的拓扑结构与文献 [Jess & Näther (2006). Inorg. Chem. 45, 7446-7454] 中报道的 CuCl(2,3-二甲基吡嗪)的两种多晶型修饰物中观察到的拓扑结构完全不同。粉末 X 射线衍射测量显示,标题化合物并不稳定,会立即转变为未知的结晶相。
Synthesis and crystal structure of poly[[μ-chlorido-μ-(2,3-dimethylpyrazine)-copper(I)] ethanol hemisolvate], which shows a new isomeric CuCl(2,3-dimethylpyrazine) network
In the crystal structure of the title compound, the copper cations are each tetrahedrally coordinated by two 2–3-dimethylpyrazine ligands and two chloride anions and linked into dinuclear units that are further connected into layers by bridging 2,3-dimethylpyrazine ligands.
Reaction of copper(I)chloride with 2,3-dimethylpyrazine in ethanol leads to the formation of the title compound, poly[[μ-chlorido-μ-(2,3-dimethylpyrazine)-copper(I)] ethanol hemisolvate], {[CuCl(C6H8N2)]·0.5C2H5OH}n or CuCl(2,3-dimethylpyrazine) ethanol hemisolvate. Its asymmetric unit consists of two crystallographically independent copper cations, two chloride anions and two 2,3-dimethylpyrazine ligands as well as one ethanol solvate molecule in general positions. The ethanol molecule is disordered and was refined using a split model. The methyl H atoms of the 2,3-dimethylpyrazine 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 tetrahedrally coordinated by two N atoms of two bridging 2,3-dimethylpyrazine ligands and two μ-1,1-bridging 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 via bridging 2,3-dimethylpyrazine coligands. These layers are stacked in such a way that channels are formed in which the disordered solvent molecules are located. The topology of this network is completely different from that observed in the two polymorphic modifications of CuCl(2,3-dimethylpyrazine) reported in the literature [Jess & Näther (2006). Inorg. Chem.45, 7446–7454]. Powder X-ray diffraction measurements reveal that the title compound is unstable and transforms immediately into an unknown crystalline phase.
期刊介绍:
Acta Crystallographica Section E: Crystallographic Communications is the IUCr''s open-access structural communications journal. It provides a fast, simple and easily accessible publication mechanism for crystal structure determinations of inorganic, metal-organic and organic compounds. The electronic submission, validation, refereeing and publication facilities of the journal ensure rapid and high-quality publication of fully validated structures. The primary article category is Research Communications; these are peer-reviewed articles describing one or more structure determinations with appropriate discussion of the science.