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":759,"journal":{"name":"Russian Journal of Coordination Chemistry","volume":"50 3","pages":"203 - 210"},"PeriodicalIF":1.1000,"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\":759,\"journal\":{\"name\":\"Russian Journal of Coordination Chemistry\",\"volume\":\"50 3\",\"pages\":\"203 - 210\"},\"PeriodicalIF\":1.1000,\"publicationDate\":\"2024-05-16\",\"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/S1070328423601437\",\"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/S1070328423601437","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CHEMISTRY, INORGANIC & NUCLEAR","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：
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.
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