Dipanjan Mondal, Sowmya Rao, Joel T. Mague, Maravanji S. Balakrishna
{"title":"半可降解二茂铁双膦配合物[Fe{C5H4P(C6H4CH2NMe2-o)2}2] Ag(I)、Au(I)、Cd(II)和Hg(II)的合成、结构表征和Hirshfeld分析","authors":"Dipanjan Mondal, Sowmya Rao, Joel T. Mague, Maravanji S. Balakrishna","doi":"10.1007/s10870-022-00966-w","DOIUrl":null,"url":null,"abstract":"<div><p>The reaction between bis(phosphino)ferrocene, [Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>-<i>o</i>)<sub>2</sub>}<sub>2</sub>] (<b>1</b>) and AgOTf resulted in disilver complex [(AgOTf)<sub>2</sub>{µ-Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>}] (<b>2</b>) which on further treatment with 2,2′-bipyrdine yielded a mixed-ligand complex [Ag<sub>2</sub>(bipy)<sub>2</sub>{µ-Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>}](OTf)<sub>2</sub> (<b>3</b>). Reaction of <b>1</b> with AuCl(SMe<sub>2</sub>) in 1:2 molar ratio afforded a digold complex [(AuCl)<sub>2</sub>Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>4</b>). Treatment of <b>4</b> with anhydrous CdCl<sub>2</sub> resulted in heterometallic complex [Fe{C<sub>5</sub>H<sub>4</sub>P(AuCl)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>(CdCl<sub>2</sub>)}<sub>2</sub>] (<b>5</b>). The reactions of <b>1</b> with anhydrous CdI<sub>2</sub> and HgI<sub>2</sub> in 1:2 molar ratios yielded bimetallic complexes [Fe{C<sub>5</sub>H<sub>4</sub>P(CdI<sub>2</sub>)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>6</b>) and [Fe{C<sub>5</sub>H<sub>4</sub>P(HgI<sub>2</sub>)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>7</b>), respectively. The molecular structures of <b>3</b>, <b>4</b> and <b>7</b> were confirmed by single crystal X-ray analysis. Complexes <b>3</b> and <b>7</b> crystallized in the triclinic space group with P-1, whereas <b>4</b> crystallized in the monoclinic space group with C2/c. Single crystals suitable for X-ray crystallography were obtained using diffusion method where a solution of [Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>1</b>) in dichloromethane was layered on a solution of CdI<sub>2</sub> and HgI<sub>2</sub> in methanol and stored at room temperature for 24 h, resulted in yellow plates of <b>6</b> and <b>7</b>, respectively. All complexes crystallized with the asymmetric unit containing half a molecule and with the Fe atom on an inversion centre. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of <b>3</b> are from H‧‧‧H (50.2%), C‧‧‧H/H‧‧‧C (8.3%), Cl‧‧‧H/H‧‧‧Cl (12.1%), O‧‧‧H/H‧‧‧O (11.3%), F‧‧‧H/H‧‧‧F (9.0%) contacts, while those for <b>4</b> are from H‧‧‧H (73.7%), C‧‧‧H/H‧‧‧C (8.9%), Cl‧‧‧H/H‧‧‧Cl (14.5%), Au‧‧‧H/H‧‧‧Au (1.8%) and N‧‧‧H/H‧‧‧N (0.8%) contacts, and those for <b>7</b> are from H‧‧‧H (65.5%), C‧‧‧H/H‧‧‧C (6.6%), I‧‧‧H/H‧‧‧I (24.1%) and I‧‧‧C/C‧‧‧I (2.9%) contacts.</p><h3>Graphical Abstract</h3><p>\n Crystal structures of silver(I), gold(I) and mercury(II) complexes containing [Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>1</b>) are described.</p><figure><div><div><div><picture><source><img></source></picture></div></div></div></figure></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"273 - 292"},"PeriodicalIF":0.4000,"publicationDate":"2022-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00966-w.pdf","citationCount":"0","resultStr":"{\"title\":\"Synthesis, Structural Characterization and Hirshfeld Analysis of Ag(I), Au(I), Cd(II) and Hg(II) Complexes Containing Hemilabile- Ferrocenylbisphosphine [Fe{C5H4P(C6H4CH2NMe2-o)2}2]\",\"authors\":\"Dipanjan Mondal, Sowmya Rao, Joel T. Mague, Maravanji S. Balakrishna\",\"doi\":\"10.1007/s10870-022-00966-w\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>The reaction between bis(phosphino)ferrocene, [Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>-<i>o</i>)<sub>2</sub>}<sub>2</sub>] (<b>1</b>) and AgOTf resulted in disilver complex [(AgOTf)<sub>2</sub>{µ-Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>}] (<b>2</b>) which on further treatment with 2,2′-bipyrdine yielded a mixed-ligand complex [Ag<sub>2</sub>(bipy)<sub>2</sub>{µ-Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>}](OTf)<sub>2</sub> (<b>3</b>). Reaction of <b>1</b> with AuCl(SMe<sub>2</sub>) in 1:2 molar ratio afforded a digold complex [(AuCl)<sub>2</sub>Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>4</b>). Treatment of <b>4</b> with anhydrous CdCl<sub>2</sub> resulted in heterometallic complex [Fe{C<sub>5</sub>H<sub>4</sub>P(AuCl)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>(CdCl<sub>2</sub>)}<sub>2</sub>] (<b>5</b>). The reactions of <b>1</b> with anhydrous CdI<sub>2</sub> and HgI<sub>2</sub> in 1:2 molar ratios yielded bimetallic complexes [Fe{C<sub>5</sub>H<sub>4</sub>P(CdI<sub>2</sub>)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>6</b>) and [Fe{C<sub>5</sub>H<sub>4</sub>P(HgI<sub>2</sub>)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>7</b>), respectively. The molecular structures of <b>3</b>, <b>4</b> and <b>7</b> were confirmed by single crystal X-ray analysis. Complexes <b>3</b> and <b>7</b> crystallized in the triclinic space group with P-1, whereas <b>4</b> crystallized in the monoclinic space group with C2/c. Single crystals suitable for X-ray crystallography were obtained using diffusion method where a solution of [Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>1</b>) in dichloromethane was layered on a solution of CdI<sub>2</sub> and HgI<sub>2</sub> in methanol and stored at room temperature for 24 h, resulted in yellow plates of <b>6</b> and <b>7</b>, respectively. All complexes crystallized with the asymmetric unit containing half a molecule and with the Fe atom on an inversion centre. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of <b>3</b> are from H‧‧‧H (50.2%), C‧‧‧H/H‧‧‧C (8.3%), Cl‧‧‧H/H‧‧‧Cl (12.1%), O‧‧‧H/H‧‧‧O (11.3%), F‧‧‧H/H‧‧‧F (9.0%) contacts, while those for <b>4</b> are from H‧‧‧H (73.7%), C‧‧‧H/H‧‧‧C (8.9%), Cl‧‧‧H/H‧‧‧Cl (14.5%), Au‧‧‧H/H‧‧‧Au (1.8%) and N‧‧‧H/H‧‧‧N (0.8%) contacts, and those for <b>7</b> are from H‧‧‧H (65.5%), C‧‧‧H/H‧‧‧C (6.6%), I‧‧‧H/H‧‧‧I (24.1%) and I‧‧‧C/C‧‧‧I (2.9%) contacts.</p><h3>Graphical Abstract</h3><p>\\n Crystal structures of silver(I), gold(I) and mercury(II) complexes containing [Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>1</b>) are described.</p><figure><div><div><div><picture><source><img></source></picture></div></div></div></figure></div>\",\"PeriodicalId\":615,\"journal\":{\"name\":\"Journal of Chemical Crystallography\",\"volume\":\"53 2\",\"pages\":\"273 - 292\"},\"PeriodicalIF\":0.4000,\"publicationDate\":\"2022-10-28\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://link.springer.com/content/pdf/10.1007/s10870-022-00966-w.pdf\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Chemical Crystallography\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://link.springer.com/article/10.1007/s10870-022-00966-w\",\"RegionNum\":4,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CRYSTALLOGRAPHY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chemical Crystallography","FirstCategoryId":"92","ListUrlMain":"https://link.springer.com/article/10.1007/s10870-022-00966-w","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CRYSTALLOGRAPHY","Score":null,"Total":0}
Synthesis, Structural Characterization and Hirshfeld Analysis of Ag(I), Au(I), Cd(II) and Hg(II) Complexes Containing Hemilabile- Ferrocenylbisphosphine [Fe{C5H4P(C6H4CH2NMe2-o)2}2]
The reaction between bis(phosphino)ferrocene, [Fe{C5H4P(C6H4CH2NMe2-o)2}2] (1) and AgOTf resulted in disilver complex [(AgOTf)2{µ-Fe{C5H4P(C6H4CH2NMe2)2}2}] (2) which on further treatment with 2,2′-bipyrdine yielded a mixed-ligand complex [Ag2(bipy)2{µ-Fe{C5H4P(C6H4CH2NMe2)2}2}](OTf)2 (3). Reaction of 1 with AuCl(SMe2) in 1:2 molar ratio afforded a digold complex [(AuCl)2Fe{C5H4P(C6H4CH2NMe2)2}2] (4). Treatment of 4 with anhydrous CdCl2 resulted in heterometallic complex [Fe{C5H4P(AuCl)(C6H4CH2NMe2)2(CdCl2)}2] (5). The reactions of 1 with anhydrous CdI2 and HgI2 in 1:2 molar ratios yielded bimetallic complexes [Fe{C5H4P(CdI2)(C6H4CH2NMe2)2}2] (6) and [Fe{C5H4P(HgI2)(C6H4CH2NMe2)2}2] (7), respectively. The molecular structures of 3, 4 and 7 were confirmed by single crystal X-ray analysis. Complexes 3 and 7 crystallized in the triclinic space group with P-1, whereas 4 crystallized in the monoclinic space group with C2/c. Single crystals suitable for X-ray crystallography were obtained using diffusion method where a solution of [Fe{C5H4P(C6H4CH2NMe2)2}2] (1) in dichloromethane was layered on a solution of CdI2 and HgI2 in methanol and stored at room temperature for 24 h, resulted in yellow plates of 6 and 7, respectively. All complexes crystallized with the asymmetric unit containing half a molecule and with the Fe atom on an inversion centre. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of 3 are from H‧‧‧H (50.2%), C‧‧‧H/H‧‧‧C (8.3%), Cl‧‧‧H/H‧‧‧Cl (12.1%), O‧‧‧H/H‧‧‧O (11.3%), F‧‧‧H/H‧‧‧F (9.0%) contacts, while those for 4 are from H‧‧‧H (73.7%), C‧‧‧H/H‧‧‧C (8.9%), Cl‧‧‧H/H‧‧‧Cl (14.5%), Au‧‧‧H/H‧‧‧Au (1.8%) and N‧‧‧H/H‧‧‧N (0.8%) contacts, and those for 7 are from H‧‧‧H (65.5%), C‧‧‧H/H‧‧‧C (6.6%), I‧‧‧H/H‧‧‧I (24.1%) and I‧‧‧C/C‧‧‧I (2.9%) contacts.
Graphical Abstract
Crystal structures of silver(I), gold(I) and mercury(II) complexes containing [Fe{C5H4P(C6H4CH2NMe2)2}2] (1) are described.
期刊介绍：
Journal of Chemical Crystallography is an international and interdisciplinary publication dedicated to the rapid dissemination of research results in the general areas of crystallography and spectroscopy. Timely research reports detail topics in crystal chemistry and physics and their relation to problems of molecular structure; structural studies of solids, liquids, gases, and solutions involving spectroscopic, spectrometric, X-ray, and electron and neutron diffraction; and theoretical studies.
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