{"title":"水合三(对氨基水杨酸)二氧铀(VI)钠的制备及晶体结构","authors":"G. Bandoli, D.A. Clemente","doi":"10.1016/0022-1902(81)80628-8","DOIUrl":null,"url":null,"abstract":"<div><p>The synthesis and crystal structure of the title compound are described. The complex crystallizes in the trigonal system, space group <em>P</em>31<em>c</em> with <em>a</em> = 16.053(12), <span><math><mtext>c = 6.839(8) </mtext><mtext>A</mtext><mtext>̊</mtext></math></span> and <em>Z</em> = 2. The structure was solved by the heavy-atom method from 1252 counter reflections, and refined by least-squares methods to <em>R</em> 0.054. Six carboxylate oxygen atoms belonging to the three nearly planar <em>p</em>-amino-salicylate ions fill the equatorial region of the linear uranyl ion, giving the <em>U</em> atom an hexagonal-bipyramidal coordination overall. The hexagon is slightly puckered (± 0.05 Å), bond lengths and angles are as expected [U-O(apical) 1.78(e), U-O(eq) 2.47(2) Å]. The exact water content (and thereafter the Na<sup>+</sup> coordination) is not entirely certain, but seems to approximate to 6H<sub>2</sub>O. The intramolecular hydrogen bond between the phenolic and a carboxylate oxygen atom, present in the free acid, is not destroyed by coordination.</p></div>","PeriodicalId":16275,"journal":{"name":"Journal of Inorganic and Nuclear Chemistry","volume":"43 11","pages":"Pages 2843-2846"},"PeriodicalIF":0.0000,"publicationDate":"1981-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0022-1902(81)80628-8","citationCount":"13","resultStr":"{\"title\":\"Preparation and crystal structure of sodium tris(p-amino-salicylato) dioxouranium(VI) hydrate\",\"authors\":\"G. Bandoli, D.A. Clemente\",\"doi\":\"10.1016/0022-1902(81)80628-8\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>The synthesis and crystal structure of the title compound are described. The complex crystallizes in the trigonal system, space group <em>P</em>31<em>c</em> with <em>a</em> = 16.053(12), <span><math><mtext>c = 6.839(8) </mtext><mtext>A</mtext><mtext>̊</mtext></math></span> and <em>Z</em> = 2. The structure was solved by the heavy-atom method from 1252 counter reflections, and refined by least-squares methods to <em>R</em> 0.054. Six carboxylate oxygen atoms belonging to the three nearly planar <em>p</em>-amino-salicylate ions fill the equatorial region of the linear uranyl ion, giving the <em>U</em> atom an hexagonal-bipyramidal coordination overall. The hexagon is slightly puckered (± 0.05 Å), bond lengths and angles are as expected [U-O(apical) 1.78(e), U-O(eq) 2.47(2) Å]. The exact water content (and thereafter the Na<sup>+</sup> coordination) is not entirely certain, but seems to approximate to 6H<sub>2</sub>O. The intramolecular hydrogen bond between the phenolic and a carboxylate oxygen atom, present in the free acid, is not destroyed by coordination.</p></div>\",\"PeriodicalId\":16275,\"journal\":{\"name\":\"Journal of Inorganic and Nuclear Chemistry\",\"volume\":\"43 11\",\"pages\":\"Pages 2843-2846\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"1981-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://sci-hub-pdf.com/10.1016/0022-1902(81)80628-8\",\"citationCount\":\"13\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Inorganic and Nuclear Chemistry\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/0022190281806288\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Inorganic and Nuclear Chemistry","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/0022190281806288","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 13
摘要
介绍了该化合物的合成方法和晶体结构。该配合物在三角形体系P31c中结晶,空间群a = 16.053(12), c = 6.839(8) Å, Z = 2。用重原子法从1252个反反射中求解该结构,并用最小二乘法将其细化为R = 0.054。6个羧酸氧原子属于3个近平面的对氨基水杨酸盐离子,填满了线性铀酰离子的赤道区,使U原子总体上呈六边形-双锥体配位。六边形略有褶皱(±0.05 Å),键长和角度与预期一致[U-O(顶端)1.78(e), U-O(eq) 2.47(2) Å]。确切的水含量(以及随后的Na+配位)不完全确定,但似乎接近6H2O。存在于游离酸中的酚和羧酸氧原子之间的分子内氢键不会被配位破坏。
Preparation and crystal structure of sodium tris(p-amino-salicylato) dioxouranium(VI) hydrate
The synthesis and crystal structure of the title compound are described. The complex crystallizes in the trigonal system, space group P31c with a = 16.053(12), and Z = 2. The structure was solved by the heavy-atom method from 1252 counter reflections, and refined by least-squares methods to R 0.054. Six carboxylate oxygen atoms belonging to the three nearly planar p-amino-salicylate ions fill the equatorial region of the linear uranyl ion, giving the U atom an hexagonal-bipyramidal coordination overall. The hexagon is slightly puckered (± 0.05 Å), bond lengths and angles are as expected [U-O(apical) 1.78(e), U-O(eq) 2.47(2) Å]. The exact water content (and thereafter the Na+ coordination) is not entirely certain, but seems to approximate to 6H2O. The intramolecular hydrogen bond between the phenolic and a carboxylate oxygen atom, present in the free acid, is not destroyed by coordination.