Christian Näther , Inke Jess , W. T. A. Harrison (Editor)
{"title":"二异硒氰四(2-甲基吡啶 N-氧化物)钴(II)和二异硒氰四(2-甲基吡啶 N-氧化物)钴(II)五倍配位和六倍配位复合物的合成及晶体结构","authors":"Christian Näther , Inke Jess , W. T. A. Harrison (Editor)","doi":"10.1107/S2056989024005073","DOIUrl":null,"url":null,"abstract":"<div><p>The crystal structures of the title compounds, which arose from the same reaction, consist of discrete complexes in which the cobalt cations are either in a CoN<sub>2</sub>O<sub>3</sub> trigonal–bipyramidal or a CoN<sub>2</sub>O<sub>4</sub> octahedral coordination.</p></div><div><p>The reaction of CoBr<sub>2</sub>, KNCSe and 2-methylpyridine <em>N</em>-oxide (C<sub>6</sub>H<sub>7</sub>NO) in ethanol leads to the formation of crystals of [Co(NCSe)<sub>2</sub>(C<sub>6</sub>H<sub>7</sub>NO)<sub>3</sub>] (<strong>1</strong>) and [Co(NCSe)<sub>2</sub>(C<sub>6</sub>H<sub>7</sub>NO)<sub>4</sub>] (<strong>2</strong>) from the same reaction mixture. The asymmetric unit of <strong>1</strong> is built up of one Co<sup>II</sup> cation, two NCSe<sup>−</sup> isoselenocyanate anions and three 2-methylpyridine <em>N</em>-oxide coligands, with all atoms located on general positions. The asymmetric unit of <strong>2</strong> consists of two cobalt cations, four isoselenocanate anions and eight 2-methylpyridine <em>N</em>-oxide coligands in general positions, because two crystallographically independent complexes are present. In compound <strong>1</strong>, the Co<sup>II</sup> cations are fivefold coordinated to two terminally N-bonded anionic ligands and three 2-methylpyridine <em>N</em>-oxide coligands within a slightly distorted trigonal–bipyramidal coordination, forming discrete complexes with the O atoms occupying the equatorial sites. In compound <strong>2</strong>, each of the two complexes is coordinated to two terminally N-bonded isoselenocyanate anions and four 2-methylpyridine <em>N</em>-oxide coligands within a slightly distorted <em>cis</em>-CoN<sub>2</sub>O<sub>4</sub> octahedral coordination geometry. In the crystal structures of <strong>1</strong> and <strong>2</strong>, the complexes are linked by weak C—H⋯Se and C—H⋯O contacts. Powder X-ray diffraction reveals that neither of the two compounds were obtained as a pure crystalline phase.</p></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 7","pages":"Pages 704-708"},"PeriodicalIF":0.5000,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Syntheses and crystal structures of the five- and sixfold coordinated complexes diisoselenocyanatotris(2-methylpyridine N-oxide)cobalt(II) and diisoselenocyanatotetrakis(2-methylpyridine N-oxide)cobalt(II)\",\"authors\":\"Christian Näther , Inke Jess , W. T. A. Harrison (Editor)\",\"doi\":\"10.1107/S2056989024005073\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>The crystal structures of the title compounds, which arose from the same reaction, consist of discrete complexes in which the cobalt cations are either in a CoN<sub>2</sub>O<sub>3</sub> trigonal–bipyramidal or a CoN<sub>2</sub>O<sub>4</sub> octahedral coordination.</p></div><div><p>The reaction of CoBr<sub>2</sub>, KNCSe and 2-methylpyridine <em>N</em>-oxide (C<sub>6</sub>H<sub>7</sub>NO) in ethanol leads to the formation of crystals of [Co(NCSe)<sub>2</sub>(C<sub>6</sub>H<sub>7</sub>NO)<sub>3</sub>] (<strong>1</strong>) and [Co(NCSe)<sub>2</sub>(C<sub>6</sub>H<sub>7</sub>NO)<sub>4</sub>] (<strong>2</strong>) from the same reaction mixture. The asymmetric unit of <strong>1</strong> is built up of one Co<sup>II</sup> cation, two NCSe<sup>−</sup> isoselenocyanate anions and three 2-methylpyridine <em>N</em>-oxide coligands, with all atoms located on general positions. The asymmetric unit of <strong>2</strong> consists of two cobalt cations, four isoselenocanate anions and eight 2-methylpyridine <em>N</em>-oxide coligands in general positions, because two crystallographically independent complexes are present. In compound <strong>1</strong>, the Co<sup>II</sup> cations are fivefold coordinated to two terminally N-bonded anionic ligands and three 2-methylpyridine <em>N</em>-oxide coligands within a slightly distorted trigonal–bipyramidal coordination, forming discrete complexes with the O atoms occupying the equatorial sites. In compound <strong>2</strong>, each of the two complexes is coordinated to two terminally N-bonded isoselenocyanate anions and four 2-methylpyridine <em>N</em>-oxide coligands within a slightly distorted <em>cis</em>-CoN<sub>2</sub>O<sub>4</sub> octahedral coordination geometry. In the crystal structures of <strong>1</strong> and <strong>2</strong>, the complexes are linked by weak C—H⋯Se and C—H⋯O contacts. Powder X-ray diffraction reveals that neither of the two compounds were obtained as a pure crystalline phase.</p></div>\",\"PeriodicalId\":7367,\"journal\":{\"name\":\"Acta Crystallographica Section E: Crystallographic Communications\",\"volume\":\"80 7\",\"pages\":\"Pages 704-708\"},\"PeriodicalIF\":0.5000,\"publicationDate\":\"2024-06-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"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/S2056989024001518\",\"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/S2056989024001518","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CRYSTALLOGRAPHY","Score":null,"Total":0}
Syntheses and crystal structures of the five- and sixfold coordinated complexes diisoselenocyanatotris(2-methylpyridine N-oxide)cobalt(II) and diisoselenocyanatotetrakis(2-methylpyridine N-oxide)cobalt(II)
The crystal structures of the title compounds, which arose from the same reaction, consist of discrete complexes in which the cobalt cations are either in a CoN2O3 trigonal–bipyramidal or a CoN2O4 octahedral coordination.
The reaction of CoBr2, KNCSe and 2-methylpyridine N-oxide (C6H7NO) in ethanol leads to the formation of crystals of [Co(NCSe)2(C6H7NO)3] (1) and [Co(NCSe)2(C6H7NO)4] (2) from the same reaction mixture. The asymmetric unit of 1 is built up of one CoII cation, two NCSe− isoselenocyanate anions and three 2-methylpyridine N-oxide coligands, with all atoms located on general positions. The asymmetric unit of 2 consists of two cobalt cations, four isoselenocanate anions and eight 2-methylpyridine N-oxide coligands in general positions, because two crystallographically independent complexes are present. In compound 1, the CoII cations are fivefold coordinated to two terminally N-bonded anionic ligands and three 2-methylpyridine N-oxide coligands within a slightly distorted trigonal–bipyramidal coordination, forming discrete complexes with the O atoms occupying the equatorial sites. In compound 2, each of the two complexes is coordinated to two terminally N-bonded isoselenocyanate anions and four 2-methylpyridine N-oxide coligands within a slightly distorted cis-CoN2O4 octahedral coordination geometry. In the crystal structures of 1 and 2, the complexes are linked by weak C—H⋯Se and C—H⋯O contacts. Powder X-ray diffraction reveals that neither of the two compounds were obtained as a pure 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.