A. Yu. Konokhova, M. Yu. Afonin, T. S. Sukhikh, S. N. Konchenko
{"title":"作为钇络合物中氨基膦酰胺配体前体的二脒膦","authors":"A. Yu. Konokhova, M. Yu. Afonin, T. S. Sukhikh, S. N. Konchenko","doi":"10.1134/S1070328423601437","DOIUrl":null,"url":null,"abstract":"<p>Diamidophosphine <sup><i>t</i></sup>BuP(NHMes)<sub>2</sub>(H<sub>2</sub>L) is synthesized by the treatment of <sup><i>t</i></sup>BuPCl<sub>2</sub> with two equivalents of KNHMes (Mes is 2,4,6-Me<sub>3</sub>C<sub>6</sub>H<sub>2</sub>). The reaction of H<sub>2</sub>L with potassium hydride in THF (THF is tetrahydrofuran) affords the anionic form HL<sup>−</sup> with the hydrogen atom migrating from nitrogen to phosphorus, which is confirmed by the <sup>1</sup>H and <sup>31</sup>P NMR data. The structure of the formed iminophosphonamidinate anion HL<sup>−</sup> is determined by X-ray diffraction (XRD) in the crystalline phase of K[K(THF)<sub>2</sub>](<sup><i>t</i></sup>BuPH(NMes)<sub>2</sub>)<sub>2</sub>∙C<sub>7</sub>H<sub>8</sub> (KHL). The reaction of KHL with yttrium chloride gives complex [Y(<sup><i>t</i></sup>BuPH(NMes)<sub>2</sub>)<sub>2</sub>Cl] ([Y(HL)<sub>2</sub>Cl]) in which, according to the XRD data, ligands HL<sup>−</sup> are in the iminophosphonamidinate PH form. The <sup>1</sup>H and <sup>31</sup>P NMR spectra confirm that this structure of the complex exists in the solution.</p>","PeriodicalId":1,"journal":{"name":"Accounts of Chemical Research","volume":null,"pages":null},"PeriodicalIF":16.4000,"publicationDate":"2024-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Diamidophosphine as a Precursor of the Iminophosphonamidinate Ligand in the Yttrium Complex\",\"authors\":\"A. Yu. Konokhova, M. Yu. Afonin, T. S. Sukhikh, S. N. Konchenko\",\"doi\":\"10.1134/S1070328423601437\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>Diamidophosphine <sup><i>t</i></sup>BuP(NHMes)<sub>2</sub>(H<sub>2</sub>L) is synthesized by the treatment of <sup><i>t</i></sup>BuPCl<sub>2</sub> with two equivalents of KNHMes (Mes is 2,4,6-Me<sub>3</sub>C<sub>6</sub>H<sub>2</sub>). The reaction of H<sub>2</sub>L with potassium hydride in THF (THF is tetrahydrofuran) affords the anionic form HL<sup>−</sup> with the hydrogen atom migrating from nitrogen to phosphorus, which is confirmed by the <sup>1</sup>H and <sup>31</sup>P NMR data. The structure of the formed iminophosphonamidinate anion HL<sup>−</sup> is determined by X-ray diffraction (XRD) in the crystalline phase of K[K(THF)<sub>2</sub>](<sup><i>t</i></sup>BuPH(NMes)<sub>2</sub>)<sub>2</sub>∙C<sub>7</sub>H<sub>8</sub> (KHL). The reaction of KHL with yttrium chloride gives complex [Y(<sup><i>t</i></sup>BuPH(NMes)<sub>2</sub>)<sub>2</sub>Cl] ([Y(HL)<sub>2</sub>Cl]) in which, according to the XRD data, ligands HL<sup>−</sup> are in the iminophosphonamidinate PH form. The <sup>1</sup>H and <sup>31</sup>P NMR spectra confirm that this structure of the complex exists in the solution.</p>\",\"PeriodicalId\":1,\"journal\":{\"name\":\"Accounts of Chemical Research\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":16.4000,\"publicationDate\":\"2024-05-16\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Accounts of Chemical Research\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://link.springer.com/article/10.1134/S1070328423601437\",\"RegionNum\":1,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Accounts of Chemical Research","FirstCategoryId":"92","ListUrlMain":"https://link.springer.com/article/10.1134/S1070328423601437","RegionNum":1,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
Diamidophosphine as a Precursor of the Iminophosphonamidinate Ligand in the Yttrium Complex
Diamidophosphine tBuP(NHMes)2(H2L) is synthesized by the treatment of tBuPCl2 with two equivalents of KNHMes (Mes is 2,4,6-Me3C6H2). The reaction of H2L with potassium hydride in THF (THF is tetrahydrofuran) affords the anionic form HL− with the hydrogen atom migrating from nitrogen to phosphorus, which is confirmed by the 1H and 31P NMR data. The structure of the formed iminophosphonamidinate anion HL− is determined by X-ray diffraction (XRD) in the crystalline phase of K[K(THF)2](tBuPH(NMes)2)2∙C7H8 (KHL). The reaction of KHL with yttrium chloride gives complex [Y(tBuPH(NMes)2)2Cl] ([Y(HL)2Cl]) in which, according to the XRD data, ligands HL− are in the iminophosphonamidinate PH form. The 1H and 31P NMR spectra confirm that this structure of the complex exists in the solution.
期刊介绍：
Accounts of Chemical Research presents short, concise and critical articles offering easy-to-read overviews of basic research and applications in all areas of chemistry and biochemistry. These short reviews focus on research from the author’s own laboratory and are designed to teach the reader about a research project. In addition, Accounts of Chemical Research publishes commentaries that give an informed opinion on a current research problem. Special Issues online are devoted to a single topic of unusual activity and significance.
Accounts of Chemical Research replaces the traditional article abstract with an article "Conspectus." These entries synopsize the research affording the reader a closer look at the content and significance of an article. Through this provision of a more detailed description of the article contents, the Conspectus enhances the article's discoverability by search engines and the exposure for the research.
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