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

IF 0.5 Q4 CRYSTALLOGRAPHY
Niklas Ruser , Christian Näther , Norbert Stock
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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.
聚μ3-乙酸-二水-μ3-硫代铈(III)的晶体结构:偶然合成具有层间O- h⋯O氢键的层状配位聚合物。
该化合物[Ce(CH3COO)(SO4)(H2O)2] n的单晶是由Ce(NO3)3·6H2O与2,5-硫代苯二酚-碳氧酸(H2TDC)和乙酸在乙醇和水的混合物中反应得到的,假设硫酸盐离子是从特氟龙反应器中浸出的,在使用前用过氧单硫酸处理过。它的不对称单元由一个CeIII阳离子、一个硫酸根离子、一个醋酸根阴离子和两个晶体独立的水分子组成,它们都位于一般位置。铈离子由三个醋酸阴离子(一个O,O螯合)和三个硫酸盐阴离子以及两个独立的水分子在不规则的CeO9配位几何结构中配位。CeIII阳离子由醋酸离子连接成[010]链,由硫酸根离子进一步连接成(001)层。观察到层内和层间的O- h⋯O氢键。粉末x射线衍射表明,只有标题化合物的痕迹与大量未知的结晶相形成。试图制备大量的标题化合物和作为纯相是不成功的。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
CiteScore
1.90
自引率
0.00%
发文量
351
审稿时长
3 weeks
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.
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