Pub Date : 2024-04-01DOI: 10.1107/S2414314624003699
Shu Hashimoto , Shintaro Miki , Tsunehisa Okuno , W. T. A. Harrison (Editor)
The cation of the title hydrated salt is a diazaborinane featuring substitution at 1, 2, and 3 positions in the nitrogen–boron six-membered heterocycle. In the crystal, the cations stack along [100] in an alternating head-to-tail manner, while the iodide ion and water molecule form one-dimensional hydrogen-bonded chains beside the cation stack. The cation stacks and I−–water chains are crosslinked by N—H⋯I and N—H⋯O hydrogen bonds.
The cation of the title hydrated salt, C17H17BN3+·I−·H2O, is a diazaborinane featuring substitution at the 1, 2, and 3 positions in the nitrogen–boron six-membered heterocycle. The cation is approximately planar with a dihedral angle between the pyridyl ring and the diazaborinane ring system of 5.40 (5)°. In the crystal, the cations stack along [100] in an alternating head-to-tail manner, while the iodide ion and water molecule form one-dimensional hydrogen-bonded chains beside the cation stack. The cation stacks and I−–water chains are crosslinked by N—H⋯I and N—H⋯O hydrogen bonds.
{"title":"4-(1H-2,3-Dihydronaphtho[1,8-de][1,3,2]diazaborinin-2-yl)-1-ethylpyridin-1-ium iodide monohydrate","authors":"Shu Hashimoto , Shintaro Miki , Tsunehisa Okuno , W. T. A. Harrison (Editor)","doi":"10.1107/S2414314624003699","DOIUrl":"10.1107/S2414314624003699","url":null,"abstract":"<div><p>The cation of the title hydrated salt is a diazaborinane featuring substitution at 1, 2, and 3 positions in the nitrogen–boron six-membered heterocycle. In the crystal, the cations stack along [100] in an alternating head-to-tail manner, while the iodide ion and water molecule form one-dimensional hydrogen-bonded chains beside the cation stack. The cation stacks and I<sup>−</sup>–water chains are crosslinked by N—H⋯I and N—H⋯O hydrogen bonds.</p></div><div><p>The cation of the title hydrated salt, C<sub>17</sub>H<sub>17</sub>BN<sub>3</sub> <sup>+</sup>·I<sup>−</sup>·H<sub>2</sub>O, is a diazaborinane featuring substitution at the 1, 2, and 3 positions in the nitrogen–boron six-membered heterocycle. The cation is approximately planar with a dihedral angle between the pyridyl ring and the diazaborinane ring system of 5.40 (5)°. In the crystal, the cations stack along [100] in an alternating head-to-tail manner, while the iodide ion and water molecule form one-dimensional hydrogen-bonded chains beside the cation stack. The cation stacks and I<sup>−</sup>–water chains are crosslinked by N—H⋯I and N—H⋯O hydrogen bonds. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (191KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11074538/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140892270","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-01DOI: 10.1107/S2414314624003468
Florian Meurer , Michael Bodensteiner , Iliyan Kolev , M. Weil (Editor)
The crystal structure model of germacrone type II determined from single-crystal X-ray data is compared with that of a previous synchrotron X-ray powder study
The extraction and purification procedures, crystallization and crystal structure refinement (single-crystal X-ray data) of germacrone type II, C15H22O, are presented. The structural results are compared with a previous powder X-ray synchrotron study [Kaduk et al. (2022#). Powder Diffr.37, 98–104], revealing significant improvements in terms of accuracy and precision. Hirshfeld atom refinement (HAR), as well as Hirshfeld surface analysis, give insight into the intermolecular interactions of germacrone type II.
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本文介绍了 C15H22O 型胚芽鞘氨醇 II 的提取和纯化过程、结晶和晶体结构（单晶 X 射线数据）的完善。结构结果与之前的粉末 X 射线同步研究[Kaduk 等人 (2022 ▸). Powder Diffr. 37, 98-104]进行了比较，发现在准确性和精确度方面都有显著提高。Hirshfeld 原子细化 (HAR) 以及 Hirshfeld 表面分析深入揭示了胚芽鞘 II 型分子间的相互作用。
{"title":"Redetermination of germacrone type II based on single-crystal X-ray data","authors":"Florian Meurer , Michael Bodensteiner , Iliyan Kolev , M. Weil (Editor)","doi":"10.1107/S2414314624003468","DOIUrl":"10.1107/S2414314624003468","url":null,"abstract":"<div><p>The crystal structure model of germacrone type II determined from single-crystal X-ray data is compared with that of a previous synchrotron X-ray powder study</p></div><div><p>The extraction and purification procedures, crystallization and crystal structure refinement (single-crystal X-ray data) of germacrone type II, C<sub>15</sub>H<sub>22</sub>O, are presented. The structural results are compared with a previous powder X-ray synchrotron study [Kaduk <em>et al.</em> (2022<span>#</span>). <em>Powder Diffr.</em> <strong>37</strong>, 98–104], revealing significant improvements in terms of accuracy and precision. Hirshfeld atom refinement (HAR), as well as Hirshfeld surface analysis, give insight into the intermolecular interactions of germacrone type II. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (238KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11074539/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140892413","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624002220
María del Consuelo Mendoza Herrera , Mario Sampedro Cruz , Lydia María Pérez Díaz , José Antonio Rivera Márquez , Laura Orea Flores , Sylvain Bernès , W. T. A. Harrison (Editor)
The chiral title compound forms supramolecular chains, through N—H⋯O hydrogen bonds between the amide and carboxylate groups.
The title molecule, C12H15NO5, is a methyl carbamate derivative obtained by reacting (R)-2-phenylglycinol and methyl chloroformate, with calcium hydroxide as heterogeneous catalyst. Supramolecular chains are formed in the [100] direction, based on N—H⋯O hydrogen bonds between the amide and carboxylate groups. These chains weakly interact in the crystal, and the phenyl rings do not display significant π–π interactions.
{"title":"Methyl N-{(1R)-2-[(methoxycarbonyl)oxy]-1-phenylethyl}carbamate","authors":"María del Consuelo Mendoza Herrera , Mario Sampedro Cruz , Lydia María Pérez Díaz , José Antonio Rivera Márquez , Laura Orea Flores , Sylvain Bernès , W. T. A. Harrison (Editor)","doi":"10.1107/S2414314624002220","DOIUrl":"10.1107/S2414314624002220","url":null,"abstract":"<div><p>The chiral title compound forms supramolecular chains, through N—H⋯O hydrogen bonds between the amide and carboxylate groups.</p></div><div><p>The title molecule, C<sub>12</sub>H<sub>15</sub>NO<sub>5</sub>, is a methyl carbamate derivative obtained by reacting (<em>R</em>)-2-phenylglycinol and methyl chloroformate, with calcium hydroxide as heterogeneous catalyst. Supramolecular chains are formed in the [100] direction, based on N—H⋯O hydrogen bonds between the amide and carboxylate groups. These chains weakly interact in the crystal, and the phenyl rings do not display significant π–π interactions. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (214KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140223552","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624001974
Jingxi Li , Sihui Long , W. T. A. Harrison (Editor)
There are two crystallographically independent molecules in the asymmetric unit of the title compound, which are linked by pairwise O—H⋯O hydrogen bonds.
The title compound, C13H10FNO2, was obtained by the reaction of 2-bromo-4-fluorobenzoic acid with aniline. There are two independent molecules, A and B, in the asymmetric unit, with slight conformational differences: the dihedral angles between the aromatic rings are 55.63 (5) and 52.65 (5)°. Both molecules feature an intramolecular N—H⋯O hydrogen bond. In the crystal, the molecules are linked by pairwise O—H⋯O hydrogen bonds to form A–B acid–acid dimers and weak C—H⋯F interactions further connect the dimers.
{"title":"4-Fluoro-2-(phenylamino)benzoic acid","authors":"Jingxi Li , Sihui Long , W. T. A. Harrison (Editor)","doi":"10.1107/S2414314624001974","DOIUrl":"10.1107/S2414314624001974","url":null,"abstract":"<div><p>There are two crystallographically independent molecules in the asymmetric unit of the title compound, which are linked by pairwise O—H⋯O hydrogen bonds.</p></div><div><p>The title compound, C<sub>13</sub>H<sub>10</sub>FNO<sub>2</sub>, was obtained by the reaction of 2-bromo-4-fluorobenzoic acid with aniline. There are two independent molecules, <em>A</em> and <em>B</em>, in the asymmetric unit, with slight conformational differences: the dihedral angles between the aromatic rings are 55.63 (5) and 52.65 (5)°. Both molecules feature an intramolecular N—H⋯O hydrogen bond. In the crystal, the molecules are linked by pairwise O—H⋯O hydrogen bonds to form <em>A</em>–<em>B</em> acid–acid dimers and weak C—H⋯F interactions further connect the dimers. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (278KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140263196","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624001895
Peter W. R. Corfield , M. Weil (Editor)
Structural analysis of the title diasteromeric sulfone determines this to be the erythro (RR/SS) isomer, and was pivotal in showing that the 1,3-elimination reactions of these compounds, which lead to substituted stilbenes, occur with inversion at each asymmetric carbon atom.
The title compound, C16H17BrO2S, crystallizes as the erythro (RR/SS) isomer of a pair of sulfones that were diastereomeric due to chirality of the α-carbon atoms on the sulfone sulfur atom. The structural analysis was pivotal in showing that the 1,3 elimination reactions of these compounds, which lead to substituted stilbenes, occur with inversion at each asymmetric carbon atom. In the crystal, C—H⋯Br and C—H⋯O hydrogen bonds link the molecules into a tri-periodic intermolecular network.
{"title":"erythro-{1-Bromo-1-[(1-phenylethyl)sulfonyl]ethyl}benzene","authors":"Peter W. R. Corfield , M. Weil (Editor)","doi":"10.1107/S2414314624001895","DOIUrl":"https://doi.org/10.1107/S2414314624001895","url":null,"abstract":"<div><p>Structural analysis of the title diasteromeric sulfone determines this to be the <em>erythro</em> (<em>RR/SS</em>) isomer, and was pivotal in showing that the 1,3-elimination reactions of these compounds, which lead to substituted stilbenes, occur with inversion at each asymmetric carbon atom.</p></div><div><p>The title compound, C<sub>16</sub>H<sub>17</sub>BrO<sub>2</sub>S, crystallizes as the <em>erythro</em> (<em>RR/SS</em>) isomer of a pair of sulfones that were diastereomeric due to chirality of the α-carbon atoms on the sulfone sulfur atom. The structural analysis was pivotal in showing that the 1,3 elimination reactions of these compounds, which lead to substituted stilbenes, occur with inversion at each asymmetric carbon atom. In the crystal, C—H⋯Br and C—H⋯O hydrogen bonds link the molecules into a tri-periodic intermolecular network. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (302KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140536247","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624002694
Layla M. Althubyani , Brian J. MacLean , Katherine N. Robertson , Manuel A.S. Aquino , M. Bolte (Editor)
The cationic complex of the title salt, [Ru(C19H13N5)2](PF6)2·3C4H10O, has the Ru atom in a slightly distorted octahedral environment of two tridentate benzimdazolyl-pyridine ligands and displays extensive π–π and C—H⋯π interactions.
The title compound, [Ru(C19H13N5)2](PF6)2·3C4H10O, was obtained from the reaction of Ru(bimpy)Cl3 [bimpy is 2,6-bis(1H-benzimidazol-2-yl)pyridine] and bimpy in refluxing ethanol followed by recrystallization from diethyl ether/acetonitrile. At 125 K the complex has orthorhombic (Pca21) symmetry. It is remarkable that the structure is almost centrosymmetric. However, refinement in space group Pbcn leads to disorder and definitely worse results. It is of interest with respect to potential catalytic reduction of CO2. The structure displays N—H⋯O, N—H⋯F hydrogen bonding and significant π–π stacking and C—H⋯π stacking interactions.
{"title":"Bis[2,6-bis(1H-benzimidazol-2-yl)pyridine]ruthenium(II) bis(hexafluoridophosphate) diethyl ether trisolvate","authors":"Layla M. Althubyani , Brian J. MacLean , Katherine N. Robertson , Manuel A.S. Aquino , M. Bolte (Editor)","doi":"10.1107/S2414314624002694","DOIUrl":"10.1107/S2414314624002694","url":null,"abstract":"<div><p>The cationic complex of the title salt, [Ru(C<sub>19</sub>H<sub>13</sub>N<sub>5</sub>)<sub>2</sub>](PF<sub>6</sub>)<sub>2</sub>·3C<sub>4</sub>H<sub>10</sub>O, has the Ru atom in a slightly distorted octahedral environment of two tridentate benzimdazolyl-pyridine ligands and displays extensive π–π and C—H⋯π interactions.</p></div><div><p>The title compound, [Ru(C<sub>19</sub>H<sub>13</sub>N<sub>5</sub>)<sub>2</sub>](PF<sub>6</sub>)<sub>2</sub>·3C<sub>4</sub>H<sub>10</sub>O, was obtained from the reaction of Ru(bimpy)Cl<sub>3</sub> [bimpy is 2,6-bis(1<em>H</em>-benzimidazol-2-yl)pyridine] and bimpy in refluxing ethanol followed by recrystallization from diethyl ether/acetonitrile. At 125 K the complex has orthorhombic (<em>Pca</em>2<sub>1</sub>) symmetry. It is remarkable that the structure is almost centrosymmetric. However, refinement in space group <em>Pbcn</em> leads to disorder and definitely worse results. It is of interest with respect to potential catalytic reduction of CO<sub>2</sub>. The structure displays N—H⋯O, N—H⋯F hydrogen bonding and significant π–π stacking and C—H⋯π stacking interactions. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (387KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140368998","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624001913
Esther H. Park , Sarah M. Ortiz , Todd K. Liang , Bradley W. Smucker , S. Bernès (Editor)
In the structure of the title compound, the Ru—N distances of the DMAP ligands are influenced by the trans chloride or dimethylsulfoxide-κS ligands.
The structure of the title compound, [RuCl2(C7H10N2)2(C2H6OS)2], has monoclinic (P21/n) symmetry. The Ru—N distances of the coordination compound are influenced by the trans chloride or dimethylsulfoxide-κS ligands. The molecular structure exhibits disorder for two of the terminal methyl groups of a dimethyl sulfoxide ligand.
{"title":"cis,cis,cis-Dichloridobis(N 4,N 4-dimethylpyridin-4-amine-κN 1)bis(dimethyl sulfoxide-κS)ruthenium(II)","authors":"Esther H. Park , Sarah M. Ortiz , Todd K. Liang , Bradley W. Smucker , S. Bernès (Editor)","doi":"10.1107/S2414314624001913","DOIUrl":"10.1107/S2414314624001913","url":null,"abstract":"<div><p>In the structure of the title compound, the Ru—N distances of the DMAP ligands are influenced by the <em>trans</em> chloride or dimethylsulfoxide-κ<em>S</em> ligands.</p></div><div><p>The structure of the title compound, [RuCl<sub>2</sub>(C<sub>7</sub>H<sub>10</sub>N<sub>2</sub>)<sub>2</sub>(C<sub>2</sub>H<sub>6</sub>OS)<sub>2</sub>], has monoclinic (<em>P</em>2<sub>1</sub>/<em>n</em>) symmetry. The Ru—N distances of the coordination compound are influenced by the <em>trans</em> chloride or dimethylsulfoxide-κ<em>S</em> ligands. The molecular structure exhibits disorder for two of the terminal methyl groups of a dimethyl sulfoxide ligand. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (270KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140077896","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The title compound was synthesized using Mn(CO)5Br. The manganese atom is situated on a crystallographic inversion center. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br and C—H⋯π interactions.
The title compound, trans-dibromidotetrakis(5-methyl-1H-pyrazole-κN2)manganese(II), [MnBr2(C4H6N2)4] or [Mn(3-MePzH)4Br2] (1) crystallizes in the triclinic P space group with the cell parameters a = 7.6288 (3), b = 8.7530 (4), c = 9.3794 (4) Å and α = 90.707 (4), β = 106.138 (4), γ = 114.285 (5)°, V = 542.62 (5) Å3, T = 120 K. The asymmetric unit contains only half the molecule with the manganese atom is situated on a crystallographic inversion center. The 3-MePzH ligands are present in an AABB type manner with two methyl groups pointing up and the other two down. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br, and C—H⋯π interactions. Earlier, a polymorphic structure of [Mn(3-MePzH)4Br2] (2) with a similar geometry and also an AABB arrangement for the pyrazole ligands was described [Reedijk et al. (1971#). Inorg. Chem. 10, 2594–2599; a = 8.802 (6), b = 9.695 (5), c = 7.613 (8) Å and α = 105.12 (4), β = 114.98 (4), γ = 92.90 (3)°, V = 558.826 (5) Å3, T = 295 K]. A varying supramolecular pattern was reported, with the structure of 1 featuring a herringbone type pattern while that of structure 2 shows a pillared network type of arrangement along the a axis. A nickel complex [Ni(3-MePzH)4Br2] isomorphic to 1 and the analogous chloro derivatives of FeII, CoII and CuII are also known.
{"title":"trans-Dibromidotetrakis(5-methyl-1H-pyrazole-κN 2)manganese(II)","authors":"Manikumar Athan , Soundararajan Krishnan , Nagarajan Loganathan , M. Zeller (Editor)","doi":"10.1107/S2414314624002372","DOIUrl":"10.1107/S2414314624002372","url":null,"abstract":"<div><p>The title compound was synthesized using Mn(CO)<sub>5</sub>Br. The manganese atom is situated on a crystallographic inversion center. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br and C—H⋯π interactions.</p></div><div><p>The title compound, <em>trans</em>-dibromidotetrakis(5-methyl-1<em>H</em>-pyrazole-κ<em>N</em> <sup>2</sup>)manganese(II), [MnBr<sub>2</sub>(C<sub>4</sub>H<sub>6</sub>N<sub>2</sub>)<sub>4</sub>] or [Mn(3-MePzH)<sub>4</sub>Br<sub>2</sub>] (<strong>1</strong>) crystallizes in the triclinic <em>P</em> <figure><img></figure> space group with the cell parameters <em>a</em> = 7.6288 (3), <em>b</em> = 8.7530 (4), <em>c</em> = 9.3794 (4) Å and α = 90.707 (4), β = 106.138 (4), γ = 114.285 (5)°, <em>V</em> = 542.62 (5) Å<sup>3</sup>, <em>T</em> = 120 K. The asymmetric unit contains only half the molecule with the manganese atom is situated on a crystallographic inversion center. The 3-MePzH ligands are present in an <em>AABB</em> type manner with two methyl groups pointing up and the other two down. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br, and C—H⋯π interactions. Earlier, a polymorphic structure of [Mn(3-MePzH)<sub>4</sub>Br<sub>2</sub>] (<strong>2</strong>) with a similar geometry and also an <em>AABB</em> arrangement for the pyrazole ligands was described [Reedijk <em>et al.</em> (1971<span>#</span>). <em>Inorg. Chem</em>. <strong>10</strong>, 2594–2599; <em>a</em> = 8.802 (6), <em>b</em> = 9.695 (5), <em>c</em> = 7.613 (8) Å and α = 105.12 (4), β = 114.98 (4), γ = 92.90 (3)°, <em>V</em> = 558.826 (5) Å<sup>3</sup>, <em>T</em> = 295 K]. A varying supramolecular pattern was reported, with the structure of <strong>1</strong> featuring a herringbone type pattern while that of structure <strong>2</strong> shows a pillared network type of arrangement along the <em>a</em> axis. A nickel complex [Ni(3-MePzH)<sub>4</sub>Br<sub>2</sub>] isomorphic to <strong>1</strong> and the analogous chloro derivatives of Fe<sup>II</sup>, Co<sup>II</sup> and Cu<sup>II</sup> are also known. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (274KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140230317","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624001755
Benjamin Knies , Ingo Hartenbach , M. Weil (Editor)
The crystal structure of defect-scheelite type Nd2/3[WO4] consists of [WO4]2− tetrahedra and trigonal [NdO8]13– dodecahedra.
Neodymium(III) ortho-oxidotungstate(VI) was synthesized as a side-product in an unsuccessful synthesis attempt at fluoride derivatives of neodymium tungstate in fused silica ampoules, using neodymium(III) oxide, neodymium(III) fluoride and tungsten trioxide. Violet, platelet-shaped single crystals of the title compound emerged of the bulk, which crystallize in the defect scheelite type with a trigonal dodecahedral coordination of oxide anions around the Nd3+ cations and the hexavalent tungsten cations situated in the centers of oxide tetrahedra.
{"title":"Crystal structure of defect scheelite-type Nd2/3[WO4]","authors":"Benjamin Knies , Ingo Hartenbach , M. Weil (Editor)","doi":"10.1107/S2414314624001755","DOIUrl":"10.1107/S2414314624001755","url":null,"abstract":"<div><p>The crystal structure of defect-scheelite type Nd<sub>2/3</sub>[WO<sub>4</sub>] consists of [WO<sub>4</sub>]<sup>2−</sup> tetrahedra and trigonal [NdO<sub>8</sub>]<sup>13–</sup> dodecahedra.</p></div><div><p>Neodymium(III) <em>ortho</em>-oxidotungstate(VI) was synthesized as a side-product in an unsuccessful synthesis attempt at fluoride derivatives of neodymium tungstate in fused silica ampoules, using neodymium(III) oxide, neodymium(III) fluoride and tungsten trioxide. Violet, platelet-shaped single crystals of the title compound emerged of the bulk, which crystallize in the defect scheelite type with a trigonal dodecahedral coordination of oxide anions around the Nd<sup>3+</sup> cations and the hexavalent tungsten cations situated in the centers of oxide tetrahedra. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (168KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140262806","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624002359
Mohd Abdul Fatah Abdul Manan , David B. Cordes , Aidan P. McKay , W. T. A. Harrison (Editor)
The crystal structure of a new fluorinated dithiocarbazate imine containing the isatin moiety, 4-fluorobenzyl (Z)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate, is described.
The title compound, C16H12FN3OS, a fluorinated dithiocarbazate imine derivative, was synthesized by the one-pot, multi-component condensation reaction of hydrazine hydrate, carbon disulfide, 4-fluorobenzyl chloride and isatin. The compound demonstrates near-planarity across much of the molecule in the solid state and a Z configuration for the azomethine C=N bond. The Z form is further stabilized by the presence of an intramolecular N—H⋯O hydrogen bond. In the extended structure, molecules are linked into dimers by N—H⋯O hydrogen bonds and further connected into chains along either [2 0] or [100] by weak C—H⋯S and C—H⋯F hydrogen bonds, which further link into corrugated sheets and in combination form the overall three-dimensional network.
{"title":"4-Fluorobenzyl (Z)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate","authors":"Mohd Abdul Fatah Abdul Manan , David B. Cordes , Aidan P. McKay , W. T. A. Harrison (Editor)","doi":"10.1107/S2414314624002359","DOIUrl":"10.1107/S2414314624002359","url":null,"abstract":"<div><p>The crystal structure of a new fluorinated dithiocarbazate imine containing the isatin moiety, 4-fluorobenzyl (<em>Z</em>)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate, is described.</p></div><div><p>The title compound, C<sub>16</sub>H<sub>12</sub>FN<sub>3</sub>OS, a fluorinated dithiocarbazate imine derivative, was synthesized by the one-pot, multi-component condensation reaction of hydrazine hydrate, carbon disulfide, 4-fluorobenzyl chloride and isatin. The compound demonstrates near-planarity across much of the molecule in the solid state and a <em>Z</em> configuration for the azomethine C=N bond. The <em>Z</em> form is further stabilized by the presence of an intramolecular N—H⋯O hydrogen bond. In the extended structure, molecules are linked into dimers by N—H⋯O hydrogen bonds and further connected into chains along either [2 <figure><img></figure> 0] or [100] by weak C—H⋯S and C—H⋯F hydrogen bonds, which further link into corrugated sheets and in combination form the overall three-dimensional network. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (225KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140228684","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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