A. N. Selikhov, G. R. Taranenko, Yu. V. Nelyubina, A. A. Trifonov
{"title":"含有三((2-二甲基氨基甲基)苯基)甲氧基配体的钾、镱(II)和钐(III)烷氧化物配合物:合成与结构","authors":"A. N. Selikhov, G. R. Taranenko, Yu. V. Nelyubina, A. A. Trifonov","doi":"10.1134/S1070328423600961","DOIUrl":null,"url":null,"abstract":"<p>The reaction of tris((2-dimethylaminomethyl)phenyl)methanol ((2-Me<sub>2</sub>NCH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>3</sub>COH) with potassium hydride in THF at –35°C affords dimeric alkoxide {[(2-Me<sub>2</sub>NCH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>3</sub>CO]K(THF)}<sub>2</sub> (<b>I</b>) in a yield of 90%. The reaction of compound <b>I</b> with YbI<sub>2</sub>(THF)<sub>2</sub> (1 : 1, 25°C) gives the Yb(II) alkoxyiodide complex {[(2-Me<sub>2</sub>NCH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>3</sub>CO]Yb(μ-I)(THF)<sub>2</sub>}<sub>2</sub> (<b>II</b>) in a yield of 57%. Complex <b>II</b> in the crystalline state is dimeric due to two bridging iodide ligands. Unlike the Yb(II) compound, the exchange reaction of complex <b>I</b> with SmI<sub>2</sub>(THF)<sub>2</sub> (1 : 1, 25°C) in THF followed by the addition of dimethoxyethane (DME) involves the oxidation of the metal to form the trivalent samarium complex [(2-Me<sub>2</sub>NCH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>3</sub>CO]<sub>2</sub>SmI (<b>III</b>), which is isolated in a yield of 60%. The molecular structures of the complexes are determined by X-ray diffraction (XRD) (CIF files CCDC nos. 2259700 (<b>I</b>), 2259701 (<b>II</b>), and 2259702 (<b>III</b>)).</p>","PeriodicalId":759,"journal":{"name":"Russian Journal of Coordination Chemistry","volume":"50 2","pages":"96 - 105"},"PeriodicalIF":1.1000,"publicationDate":"2024-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Potassium, Ytterbium(II), and Samarium(III) Alkoxide Complexes Containing the Tris((2-dimethylaminomethyl)phenyl)methoxide Ligand: Synthesis and Structures\",\"authors\":\"A. N. Selikhov, G. R. Taranenko, Yu. V. Nelyubina, A. A. Trifonov\",\"doi\":\"10.1134/S1070328423600961\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>The reaction of tris((2-dimethylaminomethyl)phenyl)methanol ((2-Me<sub>2</sub>NCH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>3</sub>COH) with potassium hydride in THF at –35°C affords dimeric alkoxide {[(2-Me<sub>2</sub>NCH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>3</sub>CO]K(THF)}<sub>2</sub> (<b>I</b>) in a yield of 90%. The reaction of compound <b>I</b> with YbI<sub>2</sub>(THF)<sub>2</sub> (1 : 1, 25°C) gives the Yb(II) alkoxyiodide complex {[(2-Me<sub>2</sub>NCH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>3</sub>CO]Yb(μ-I)(THF)<sub>2</sub>}<sub>2</sub> (<b>II</b>) in a yield of 57%. Complex <b>II</b> in the crystalline state is dimeric due to two bridging iodide ligands. Unlike the Yb(II) compound, the exchange reaction of complex <b>I</b> with SmI<sub>2</sub>(THF)<sub>2</sub> (1 : 1, 25°C) in THF followed by the addition of dimethoxyethane (DME) involves the oxidation of the metal to form the trivalent samarium complex [(2-Me<sub>2</sub>NCH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>3</sub>CO]<sub>2</sub>SmI (<b>III</b>), which is isolated in a yield of 60%. The molecular structures of the complexes are determined by X-ray diffraction (XRD) (CIF files CCDC nos. 2259700 (<b>I</b>), 2259701 (<b>II</b>), and 2259702 (<b>III</b>)).</p>\",\"PeriodicalId\":759,\"journal\":{\"name\":\"Russian Journal of Coordination Chemistry\",\"volume\":\"50 2\",\"pages\":\"96 - 105\"},\"PeriodicalIF\":1.1000,\"publicationDate\":\"2024-05-08\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Russian Journal of Coordination Chemistry\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://link.springer.com/article/10.1134/S1070328423600961\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CHEMISTRY, INORGANIC & NUCLEAR\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Russian Journal of Coordination Chemistry","FirstCategoryId":"92","ListUrlMain":"https://link.springer.com/article/10.1134/S1070328423600961","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CHEMISTRY, INORGANIC & NUCLEAR","Score":null,"Total":0}
引用次数: 0
摘要
摘要三((2-二甲基氨基甲基)苯基)甲醇((2-Me2NCH2C6H4)3COH)与氢化钾在 THF 中于 -35°C 反应生成二聚烷氧基化合物 {[(2-Me2NCH2C6H4)3CO]K(THF)}2 (I),产率为 90%。化合物 I 与 YbI2(THF)2(1:1,25°C)反应生成 Yb(II)烷氧基碘化物络合物 {[(2-Me2NCH2C6H4)3CO]Yb(μ-I)(THF)2}2 (II),产率为 57%。由于存在两个桥接碘配体,晶体态的络合物 II 是二聚体。与 Yb(II) 化合物不同,络合物 I 与 SmI2(THF)2 (1:1,25°C)在 THF 中发生交换反应,然后加入二甲氧基乙烷 (DME),金属被氧化,形成三价钐络合物 [(2-Me2NCH2C6H4)3CO]2SmI (III),该络合物的分离率为 60%。复合物的分子结构是通过 X 射线衍射(XRD)确定的(CIF 文件 CCDC 编号:2259700(I)、2259701(II)和 2259702(III))。
Potassium, Ytterbium(II), and Samarium(III) Alkoxide Complexes Containing the Tris((2-dimethylaminomethyl)phenyl)methoxide Ligand: Synthesis and Structures
The reaction of tris((2-dimethylaminomethyl)phenyl)methanol ((2-Me2NCH2C6H4)3COH) with potassium hydride in THF at –35°C affords dimeric alkoxide {[(2-Me2NCH2C6H4)3CO]K(THF)}2 (I) in a yield of 90%. The reaction of compound I with YbI2(THF)2 (1 : 1, 25°C) gives the Yb(II) alkoxyiodide complex {[(2-Me2NCH2C6H4)3CO]Yb(μ-I)(THF)2}2 (II) in a yield of 57%. Complex II in the crystalline state is dimeric due to two bridging iodide ligands. Unlike the Yb(II) compound, the exchange reaction of complex I with SmI2(THF)2 (1 : 1, 25°C) in THF followed by the addition of dimethoxyethane (DME) involves the oxidation of the metal to form the trivalent samarium complex [(2-Me2NCH2C6H4)3CO]2SmI (III), which is isolated in a yield of 60%. The molecular structures of the complexes are determined by X-ray diffraction (XRD) (CIF files CCDC nos. 2259700 (I), 2259701 (II), and 2259702 (III)).
期刊介绍:
Russian Journal of Coordination Chemistry is a journal that publishes reviews, original papers, and short communications on all aspects of theoretical and experimental coordination chemistry. Modern coordination chemistry is an interdisciplinary science that makes a bridge between inorganic, organic, physical, analytical, and biological chemistry.