A. E. Zazulya, P. A. Abramov, S. V. Tkachev, D. G. Sheven’, A. Yu. Komarovskikh, P. E. Plyusnin, D. B. Vasilchenko
{"title":"反式、反式-[Pt(py)2(N3)2(OH)2]·2H2O的结构及基于它的Pt(IV)前药的合成","authors":"A. E. Zazulya, P. A. Abramov, S. V. Tkachev, D. G. Sheven’, A. Yu. Komarovskikh, P. E. Plyusnin, D. B. Vasilchenko","doi":"10.1134/S0022476625090057","DOIUrl":null,"url":null,"abstract":"<p>The structure of <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)<sub>2</sub>]·2H<sub>2</sub>O is studied by single crystal X-ray diffraction. The crystallographic data are: <i>a</i> = 9.8240(2) Å, <i>b</i> = 17.2178(3) Å, <i>c</i> = 9.5248(2) Å, β = 97.777(1)°, space group <i>P</i>2<sub>1</sub>/<i>c</i>, <i>Z</i> = 4, ρ<sub>cal</sub> = 2.11 g/cm<sup>3</sup>. The crystal structure of the complex consists of molecular layers perpendicular to the <i>c</i> direction. The transformation process of the dehydrate to the anhydrous complex is analyzed by thermal gravimetry. The previously published synthesis procedures of <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)(SuccH)] and <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)(Succ-NH-TEMPO)] complexes from <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)<sub>2</sub>] are modified. The optimization of synthesis conditions and the product isolation procedure increases the product yield and substantially improves the purity of the obtained compounds.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1820 - 1830"},"PeriodicalIF":1.4000,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Structure of trans,trans-[Pt(py)2(N3)2(OH)2]·2H2O and Synthesis of Pt(IV) Prodrugs Based on It\",\"authors\":\"A. E. Zazulya, P. A. Abramov, S. V. Tkachev, D. G. Sheven’, A. Yu. Komarovskikh, P. E. Plyusnin, D. B. Vasilchenko\",\"doi\":\"10.1134/S0022476625090057\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>The structure of <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)<sub>2</sub>]·2H<sub>2</sub>O is studied by single crystal X-ray diffraction. The crystallographic data are: <i>a</i> = 9.8240(2) Å, <i>b</i> = 17.2178(3) Å, <i>c</i> = 9.5248(2) Å, β = 97.777(1)°, space group <i>P</i>2<sub>1</sub>/<i>c</i>, <i>Z</i> = 4, ρ<sub>cal</sub> = 2.11 g/cm<sup>3</sup>. The crystal structure of the complex consists of molecular layers perpendicular to the <i>c</i> direction. The transformation process of the dehydrate to the anhydrous complex is analyzed by thermal gravimetry. The previously published synthesis procedures of <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)(SuccH)] and <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)(Succ-NH-TEMPO)] complexes from <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)<sub>2</sub>] are modified. The optimization of synthesis conditions and the product isolation procedure increases the product yield and substantially improves the purity of the obtained compounds.</p>\",\"PeriodicalId\":668,\"journal\":{\"name\":\"Journal of Structural Chemistry\",\"volume\":\"66 9\",\"pages\":\"1820 - 1830\"},\"PeriodicalIF\":1.4000,\"publicationDate\":\"2025-10-09\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Structural Chemistry\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://link.springer.com/article/10.1134/S0022476625090057\",\"RegionNum\":4,\"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":"Journal of Structural Chemistry","FirstCategoryId":"92","ListUrlMain":"https://link.springer.com/article/10.1134/S0022476625090057","RegionNum":4,"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
用单晶x射线衍射研究了反式,反式-[Pt(py)2(N3)2(OH)2]·2H2O的结构。晶体数据:= 9.8240 (2)a, b = 17.2178 (3) a, c = 9.5248(2),β= 97.777(1)°,空间群P21 / c、Z = 4,ρ卡尔= 2.11克/立方厘米。该配合物的晶体结构由垂直于c方向的分子层组成。用热重法分析了脱水产物向无水络合物的转变过程。对先前发表的由trans,trans-[Pt(py)2(N3)2(OH)2]合成的trans,trans-[Pt(py)2(N3)2(OH)2]和trans,trans-[Pt(py)2(N3)2(OH)2] (ske - nh - tempo)]配合物进行了改进。合成条件和产物分离工艺的优化提高了产物得率,大大提高了所得化合物的纯度。
Structure of trans,trans-[Pt(py)2(N3)2(OH)2]·2H2O and Synthesis of Pt(IV) Prodrugs Based on It
The structure of trans,trans-[Pt(py)2(N3)2(OH)2]·2H2O is studied by single crystal X-ray diffraction. The crystallographic data are: a = 9.8240(2) Å, b = 17.2178(3) Å, c = 9.5248(2) Å, β = 97.777(1)°, space group P21/c, Z = 4, ρcal = 2.11 g/cm3. The crystal structure of the complex consists of molecular layers perpendicular to the c direction. The transformation process of the dehydrate to the anhydrous complex is analyzed by thermal gravimetry. The previously published synthesis procedures of trans,trans-[Pt(py)2(N3)2(OH)(SuccH)] and trans,trans-[Pt(py)2(N3)2(OH)(Succ-NH-TEMPO)] complexes from trans,trans-[Pt(py)2(N3)2(OH)2] are modified. The optimization of synthesis conditions and the product isolation procedure increases the product yield and substantially improves the purity of the obtained compounds.
期刊介绍:
Journal is an interdisciplinary publication covering all aspects of structural chemistry, including the theory of molecular structure and chemical bond; the use of physical methods to study the electronic and spatial structure of chemical species; structural features of liquids, solutions, surfaces, supramolecular systems, nano- and solid materials; and the crystal structure of solids.