{"title":"Crystal structure of poly[μ3-acetato-diaqua-μ3-sulfato-cerium(III)]: serendipitous synthesis of a layered coordination polymer exhibiting interlayer O—H⋯O hydrogen bonding","authors":"Niklas Ruser , Christian Näther , Norbert Stock","doi":"10.1107/S2056989024012313","DOIUrl":null,"url":null,"abstract":"<div><div>In the crystal structure of the title compound, the Ce<sup>III</sup> cations are ninefold coordinated and linked into chains <em>via</em> the acetate anions and are further connected into layers by the sulfate dianions.</div></div><div><div>Single crystals of the title compound, [Ce(CH<sub>3</sub>COO)(SO<sub>4</sub>)(H<sub>2</sub>O)<sub>2</sub>]<sub><em>n</em></sub>, were obtained serendipitously by the reaction of Ce(NO<sub>3</sub>)<sub>3</sub>·6H<sub>2</sub>O with 2,5-thiophenedicarboxylic acid (H<sub>2</sub>TDC) and acetic acid in a mixture of ethanol and water, where it is assumed that the sulfate ions leached from the Teflon reactor, which was treated with peroxymonosulfuric acid prior to its use. Its asymmetric unit consists of one Ce<sup>III</sup> cation, one sulfate dianion, one acetate anion and two crystallographically independent water molecules, all of them located in general positions. The cerium cations are coordinated by three acetate anions (one <em>O</em>,<em>O</em>-chelating) and three sulfate dianions that are related by symmetry as well as two independent water molecules within an irregular CeO<sub>9</sub> coordination geometry. The Ce<sup>III</sup> cations are linked by the acetate ions into [010] chains, which are further connected into (001) layers by the sulfate dianions. Intralayer and interlayer O—H⋯O hydrogen bonds are observed. Powder X-ray diffraction shows that only traces of the title compound have formed together with a large amount of an unknown crystalline phase. Attempts to prepare the title compound in larger amounts and as a pure phase were unsuccessful.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 2","pages":"Pages 104-108"},"PeriodicalIF":0.5000,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11799791/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/S2056989025000222","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
Abstract
In the crystal structure of the title compound, the CeIII cations are ninefold coordinated and linked into chains via the acetate anions and are further connected into layers by the sulfate dianions.
Single crystals of the title compound, [Ce(CH3COO)(SO4)(H2O)2]n, were obtained serendipitously by the reaction of Ce(NO3)3·6H2O with 2,5-thiophenedicarboxylic acid (H2TDC) and acetic acid in a mixture of ethanol and water, where it is assumed that the sulfate ions leached from the Teflon reactor, which was treated with peroxymonosulfuric acid prior to its use. Its asymmetric unit consists of one CeIII cation, one sulfate dianion, one acetate anion and two crystallographically independent water molecules, all of them located in general positions. The cerium cations are coordinated by three acetate anions (one O,O-chelating) and three sulfate dianions that are related by symmetry as well as two independent water molecules within an irregular CeO9 coordination geometry. The CeIII cations are linked by the acetate ions into [010] chains, which are further connected into (001) layers by the sulfate dianions. Intralayer and interlayer O—H⋯O hydrogen bonds are observed. Powder X-ray diffraction shows that only traces of the title compound have formed together with a large amount of an unknown crystalline phase. Attempts to prepare the title compound in larger amounts and as a pure phase were unsuccessful.
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.