Pub Date : 2025-12-01DOI: 10.1107/S2056989025010400
Reham A. Mohamed-Ezzat , Galal H. Elgemeie , Peter G. Jones
The (modified) triazine ring in the title compound is planar. The packing involves classical and ‘weak’ hydrogen bonds, together with π contacts to the triazine ring.
In the structure of the title compound, C23H20ClN5O4S2·2C2H6OS, the two DMSO solvent molecules are hydrogen bonded to the two NH groups of the main molecule. The (modified) triazine ring is planar and is approximately perpendicular to its directly bonded methoxyphenyl substituent. The bond lengths and angles indicate extensive delocalization of the multiple bonding. The packing is characterized by a large number of borderline contacts, especially ‘weak’ hydrogen bonds. There is no π–π stacking. The centroid of the triazine ring is involved in two short contacts, namely 2.63 Å to a phenyl hydrogen atom and 3.0509 (9) Å to a methoxy oxygen atom.
{"title":"Crystal structure of 4-chloro-N-{5-(4-methoxyphenyl)-4-[(4-methoxyphenyl)amino]-6-sulfanylidene-1,2,5,6-tetrahydro-1,3,5-triazin-2-ylidene}benzenesulfonamide dimethyl sulfoxide disolvate","authors":"Reham A. Mohamed-Ezzat , Galal H. Elgemeie , Peter G. Jones","doi":"10.1107/S2056989025010400","DOIUrl":"10.1107/S2056989025010400","url":null,"abstract":"<div><div>The (modified) triazine ring in the title compound is planar. The packing involves classical and ‘weak’ hydrogen bonds, together with π contacts to the triazine ring.</div></div><div><div>In the structure of the title compound, C<sub>23</sub>H<sub>20</sub>ClN<sub>5</sub>O<sub>4</sub>S<sub>2</sub>·2C<sub>2</sub>H<sub>6</sub>OS, the two DMSO solvent molecules are hydrogen bonded to the two NH groups of the main molecule. The (modified) triazine ring is planar and is approximately perpendicular to its directly bonded methoxyphenyl substituent. The bond lengths and angles indicate extensive delocalization of the multiple bonding. The packing is characterized by a large number of borderline contacts, especially ‘weak’ hydrogen bonds. There is no π–π stacking. The centroid of the triazine ring is involved in two short contacts, namely 2.63 Å to a phenyl hydrogen atom and 3.0509 (9) Å to a methoxy oxygen atom.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 12","pages":"Pages 1178-1181"},"PeriodicalIF":0.6,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145754041","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
In the complex anion in the title compound, the cerium cation adopts a near regular square-antiprismatic coordination geometry arising from four O,O-bidentate ligands.
The title compound, (C8H10N3)[Ce(C7H3F3NO2S)4], crystallizes with two cations and two anions in the asymmetric unit, with ion pairs linked by N—H⋯O hydrogen bonds. The Ce3+ cations adopt near regular square-antiprismatic coordination geometries, arising from four O,O-bidentate ligands. Numerous N—H⋯F hydrogen bonds, as well as weak contacts such as C—H⋯F and C—H⋯N interactions occur in the extended structure. Hirshfeld surface analysis indicates that 34.8% of intermolecular interactions are attributed to F⋯H/H⋯F, 13.2% to H⋯C/C⋯H, 11.1% to H⋯H, 6.6% to H⋯S/S⋯H and 5.5% to H⋯O/O⋯H contacts.
{"title":"Synthesis and structure of 2-amino-1-methylbenzimidazolium tetrakis[4,4,4-trifluoro-1-(1,3-thiazol-2-yl)butane-1,3-dionato-κ2O,O′]cerium(III)","authors":"Feruza Fayzullayeva , Sardor Murodov , Kambarali Turgunov , Mushtariybegim Sunnatillayeva , Bakhtigul Ruzieva , Bakhodir Tashkhodjaev , Shakhlo Daminova","doi":"10.1107/S2056989025010266","DOIUrl":"10.1107/S2056989025010266","url":null,"abstract":"<div><div>In the complex anion in the title compound, the cerium cation adopts a near regular square-antiprismatic coordination geometry arising from four O,O-bidentate ligands.</div></div><div><div>The title compound, (C<sub>8</sub>H<sub>10</sub>N<sub>3</sub>)[Ce(C<sub>7</sub>H<sub>3</sub>F<sub>3</sub>NO<sub>2</sub>S)<sub>4</sub>], crystallizes with two cations and two anions in the asymmetric unit, with ion pairs linked by N—H⋯O hydrogen bonds. The Ce<sup>3+</sup> cations adopt near regular square-antiprismatic coordination geometries, arising from four <em>O</em>,<em>O</em>-bidentate ligands. Numerous N—H⋯F hydrogen bonds, as well as weak contacts such as C—H⋯F and C—H⋯N interactions occur in the extended structure. Hirshfeld surface analysis indicates that 34.8% of intermolecular interactions are attributed to F⋯H/H⋯F, 13.2% to H⋯C/C⋯H, 11.1% to H⋯H, 6.6% to H⋯S/S⋯H and 5.5% to H⋯O/O⋯H contacts.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 12","pages":"Pages 1164-1169"},"PeriodicalIF":0.6,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145754125","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A one-dimensional lanthanum coordination polymer based on 3,6-dichlorophthalate has been prepared by microwaves-assisted synthesis and structurally described.
A one-dimensional lanthanum-based coordination polymer based on 3,6-dichlorophthalate has been prepared and structurally described, namely, poly[[tetraaqua[2,4-dichloro-6-(ethoxycarbonyl)benzoato](μ3-3,6-dichlorophthalato)lanthanum(III)] monohydrate], {[La(C8H2Cl2O4)(C10H7Cl2O4)(H2O)4]·H2O}∞. Its crystal structure can be described based on molecular double chains in which lanthanum ions are linked to each other by ligands. There are several structural features that seem promising as far as luminescence properties are concerned, such as the presence of strong hydrogen bonds and of short halogen contacts, as well as quite long intermetallic distances. It is a pity that, to date, only a lanthanum-based compound has been obtained.
{"title":"A lanthanum coordination polymer with 3,6-dichlorophthalate and 2,4-dichloro-6-(ethoxycarbonyl)benzoate as ligands","authors":"Christine Hénaff , Thierry Roisnel , Chloé Blais , Olivier Guillou , Carole Daiguebonne","doi":"10.1107/S2056989025009508","DOIUrl":"10.1107/S2056989025009508","url":null,"abstract":"<div><div>A one-dimensional lanthanum coordination polymer based on 3,6-dichlorophthalate has been prepared by microwaves-assisted synthesis and structurally described.</div></div><div><div>A one-dimensional lanthanum-based coordination polymer based on 3,6-dichlorophthalate has been prepared and structurally described, namely, poly[[tetraaqua[2,4-dichloro-6-(ethoxycarbonyl)benzoato](μ<sub>3</sub>-3,6-dichlorophthalato)lanthanum(III)] monohydrate], {[La(C<sub>8</sub>H<sub>2</sub>Cl<sub>2</sub>O<sub>4</sub>)(C<sub>10</sub>H<sub>7</sub>Cl<sub>2</sub>O<sub>4</sub>)(H<sub>2</sub>O)<sub>4</sub>]·H<sub>2</sub>O}<sub>∞</sub>. Its crystal structure can be described based on molecular double chains in which lanthanum ions are linked to each other by ligands. There are several structural features that seem promising as far as luminescence properties are concerned, such as the presence of strong hydrogen bonds and of short halogen contacts, as well as quite long intermetallic distances. It is a pity that, to date, only a lanthanum-based compound has been obtained.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 12","pages":"Pages 1106-1110"},"PeriodicalIF":0.6,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145754135","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-01DOI: 10.1107/S2056989025009740
Mohamed Ait Idar , Yousri El Barkaoui , Tuncer Hökelek , Olivier Blacque , Hassan Cherkaoui , Ahmed Moussaif
In the hydrated title compound, two substituted benzimidazole ring systems are bridged over a pyridine ring. O—H—N and C—H—O hydrogen bonds as well as π–π stacking interactions consolidate the crystal packing.
The title compound, C25H17N5·0.144H2O, contains two substituted benzimidazole ring systems bridged over a pyridine ring and a disordered non-coordinating water molecule. In the crystal, O—H⋯N and C—H⋯O hydrogen-bonding interactions link the molecules into infinite chains parallel to [101]. Furthermore, π–π stacking interactions between the imidazole rings and between the pyridine and imidazole rings of adjacent molecules with inter-centroid distances of 3.6371 (4), 3.9872 (5), 3.4916 (4) and 3.6648 (4) Å are present, but C—H⋯π(ring) interactions are not observed. Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (39.3%), H⋯C/C⋯H (35.9%) and H⋯N/N⋯H (9.1%).
{"title":"Crystal structure and Hirshfeld surface analysis of 2,6-bis[1-(prop-2-yn-1-yl)-1H-benzo[d]imidazol-2-yl]pyridine 0.144-hydrate","authors":"Mohamed Ait Idar , Yousri El Barkaoui , Tuncer Hökelek , Olivier Blacque , Hassan Cherkaoui , Ahmed Moussaif","doi":"10.1107/S2056989025009740","DOIUrl":"10.1107/S2056989025009740","url":null,"abstract":"<div><div>In the hydrated title compound, two substituted benzimidazole ring systems are bridged over a pyridine ring. O—H—N and C—H—O hydrogen bonds as well as π–π stacking interactions consolidate the crystal packing.</div></div><div><div>The title compound, C<sub>25</sub>H<sub>17</sub>N<sub>5</sub>·0.144H<sub>2</sub>O, contains two substituted benzimidazole ring systems bridged over a pyridine ring and a disordered non-coordinating water molecule. In the crystal, O—H⋯N and C—H⋯O hydrogen-bonding interactions link the molecules into infinite chains parallel to [101]. Furthermore, π–π stacking interactions between the imidazole rings and between the pyridine and imidazole rings of adjacent molecules with inter-centroid distances of 3.6371 (4), 3.9872 (5), 3.4916 (4) and 3.6648 (4) Å are present, but C—H⋯π(ring) interactions are not observed. Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (39.3%), H⋯C/C⋯H (35.9%) and H⋯N/N⋯H (9.1%).</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 12","pages":"Pages 1126-1130"},"PeriodicalIF":0.6,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145754038","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-01DOI: 10.1107/S2056989025009867
A. M. Buddhika Chandima , Stanislav Groysman , Cassandra L. Ward
Treatment of a tetra(acetonitrile)copper(I) precursor with excess xylyl isocyanide forms the title tetra(isocyanide)copper(I) complex, which was characterized structurally and spectroscopically.
Treatment of the CuI precursor [Cu(NCMe)4]PF6 with excess (10 equivalents) of relatively bulky xylyl isocyanide formed a tetra(isocyanide) complex, namely, tetrakis(2,6-dimethylphenylisocyanide)copper(I) hexafluorophosphate, [Cu(C9H9N)4]PF6 or [Cu(CNXyl)4]PF6, in good yield. This is in contrast to the previously reported reactions of CuI precursors with approximately three equivalents of xylyl isocyanide, which led selectively to the formation of tris(isocyanide) complexes. The copper atom lies on a twofold axis and P atom on an inversion centre. The complex was characterized by X-ray crystallography, IR spectroscopy, and 1H/13C {1H} NMR spectroscopy. In the crystal structure, each individual [Cu(CNXyl)4]+ molecule demonstrates two pairs of coplanar xylyl isocyanide ligands. This arrangement leads to intermolecular π-stacking interactions between nearby complex molecules.
四（乙腈）-铜(I)前驱体与过量异氰酸二酯处理形成标题四（异氰酸）铜(I)配合物，并对其进行了结构和光谱表征。将CuI前驱体[Cu(NCMe)4]PF6用过量的（10等量）相对较大的二甲苯异氰酸酯处理形成四（异氰酸酯）络合物，即四- kis -（2,6-二甲基苯基异氰酸酯）铜(I)六氟磷酸，[Cu(C9H9N)4]PF6或[Cu(CNX-yl)4]PF6，收率很高。这与先前报道的CuI前体与大约三个等量的异氰酸二甲苯的反应形成对比，后者导致选择性地形成三（异氰酸二甲苯）络合物。铜原子位于双轴上，P原子位于反转中心上。通过x射线晶体学、红外光谱和1H/13C {1H}核磁共振光谱对配合物进行了表征。在晶体结构中，每个[Cu(CNX-yl)4]+分子具有两对共面异氰酸二酯配体。这种排列导致附近复杂分子之间的分子间π堆积相互作用。
{"title":"Synthesis and structure of a tetrahedral homoleptic CuI complex with xylyl isocyanide","authors":"A. M. Buddhika Chandima , Stanislav Groysman , Cassandra L. Ward","doi":"10.1107/S2056989025009867","DOIUrl":"10.1107/S2056989025009867","url":null,"abstract":"<div><div>Treatment of a tetra(acetonitrile)copper(I) precursor with excess xylyl isocyanide forms the title tetra(isocyanide)copper(I) complex, which was characterized structurally and spectroscopically.</div></div><div><div>Treatment of the Cu<sup>I</sup> precursor [Cu(NCMe)<sub>4</sub>]PF<sub>6</sub> with excess (10 equivalents) of relatively bulky xylyl isocyanide formed a tetra(isocyanide) complex, namely, tetrakis(2,6-dimethylphenylisocyanide)copper(I) hexafluorophosphate, [Cu(C<sub>9</sub>H<sub>9</sub>N)<sub>4</sub>]PF<sub>6</sub> or [Cu(CNXyl)<sub>4</sub>]PF<sub>6</sub>, in good yield. This is in contrast to the previously reported reactions of Cu<sup>I</sup> precursors with approximately three equivalents of xylyl isocyanide, which led selectively to the formation of tris(isocyanide) complexes. The copper atom lies on a twofold axis and P atom on an inversion centre. The complex was characterized by X-ray crystallography, IR spectroscopy, and <sup>1</sup>H/<sup>13</sup>C {<sup>1</sup>H} NMR spectroscopy. In the crystal structure, each individual [Cu(CNXyl)<sub>4</sub>]<sup>+</sup> molecule demonstrates two pairs of coplanar xylyl isocyanide ligands. This arrangement leads to intermolecular π-stacking interactions between nearby complex molecules.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 12","pages":"Pages 1153-1157"},"PeriodicalIF":0.6,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145754124","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-01DOI: 10.1107/S2056989025010060
Jose de Jesus Velazquez-Garcia , Christos Bintas , Faegheh Khademhir , Bassima Knjo , Aliyenur Ekineken , Fabienne Hain , Simone Techert
The structure of a tris[hexakis(imidazole)cobalt(II)] bis(benzene-1,3,5-tricarboxylate) compound was determined by single-crystal X-ray diffraction.
The title compound, [CoII(C3H4N2)6]3(C9H3O6)2 (1), was synthesized from cobalt chloride(II), benzene-1,3,5-tricarboxylic acid (H3btc) and imidazole (Im) in an ethanol/DMF mixture via slow evaporation at room temperature. This compound consists of three hexakis(imidazole)cobalt(II) cations and two trimesate anions. Examination of the crystal packing shows the formation of one-dimensional stacks of ions propagating along the c axis. The packing interactions are primarily driven by N—H⋯O hydrogen bonding between anions and cations.
{"title":"Crystal structure of tris[hexakis(imidazole)cobalt(II)] bis(benzene-1,3,5-tricarboxylate)","authors":"Jose de Jesus Velazquez-Garcia , Christos Bintas , Faegheh Khademhir , Bassima Knjo , Aliyenur Ekineken , Fabienne Hain , Simone Techert","doi":"10.1107/S2056989025010060","DOIUrl":"10.1107/S2056989025010060","url":null,"abstract":"<div><div>The structure of a tris[hexakis(imidazole)cobalt(II)] bis(benzene-1,3,5-tricarboxylate) compound was determined by single-crystal X-ray diffraction.</div></div><div><div>The title compound, [Co<sup>II</sup>(C<sub>3</sub>H<sub>4</sub>N<sub>2</sub>)<sub>6</sub>]<sub>3</sub>(C<sub>9</sub>H<sub>3</sub>O<sub>6</sub>)<sub>2</sub> (<strong>1</strong>), was synthesized from cobalt chloride(II), benzene-1,3,5-tricarboxylic acid (H<sub>3</sub>btc) and imidazole (Im) in an ethanol/DMF mixture <em>via</em> slow evaporation at room temperature. This compound consists of three hexakis(imidazole)cobalt(II) cations and two trimesate anions. Examination of the crystal packing shows the formation of one-dimensional stacks of ions propagating along the <em>c</em> axis. The packing interactions are primarily driven by N—H⋯O hydrogen bonding between anions and cations.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 12","pages":"Pages 1186-1188"},"PeriodicalIF":0.6,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145754132","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-01DOI: 10.1107/S205698902500920X
Clifford W. Padgett , Will E. Lynch , Stephen N. Crooke , Christine R. Whitlock
In the title solvates, the indole ring rotations (58–72°) relative to the plane of the central ring govern non-planarity. In the extended structures, N—H⋯O links form chains or sheets and disordered solvents were masked.
The syntheses and structures of the dimethyl sulfoxide (DMSO) solvate of 3,6-bis(indol-3-yl)-1,4-dimethylpiperazine-2,5-dione, C11H10N2O (I), and of the dimethyl sulfoxide and tetrahydrofuran (THF) solvates of 1,4-dimethyl-3,6-bis(2-methylindol-3-yl)piperazine-2,5-dione, C12H12N2O, (II) and (III), respectively, are reported. The asymmetric units of (I) and (II) each contain two crystallographically independent half-molecules that are completed by inversion symmetry, whereas (III) contains one independent half-molecule. In all three structures, the piperazine-2,5-dione core is essentially planar and the overall molecular non-planarity arises from rotations of the indole substituents: ranging between 58 and 63° in (I), approximately 72° for both independent molecules in (II) and approximately 62° in (III). In the crystal of (I), molecules are linked by two N—H⋯O hydrogen bonds to form C(18) chains; (II) features a single N—H⋯O contact giving C(8) chains; and (III) exhibits N—H⋯O interactions that generate C(7) chains assembling into sheets lying parallel to (100). No significant π–π stacking is present in any of these structures. All three structures contain regions of disordered solvent (DMSO or THF) that were treated with a solvent mask during refinement.
{"title":"Crystal structures of the dimethyl sulfoxide solvate of 3,6-bis(indol-3-yl)-1,4-dimethylpiperazine-2,5-dione and of the dimethyl sulfoxide and tetrahydrofuran solvates of 1,4-dimethyl-3,6-bis(2-methylindol-3-yl)piperazine-2,5-dione","authors":"Clifford W. Padgett , Will E. Lynch , Stephen N. Crooke , Christine R. Whitlock","doi":"10.1107/S205698902500920X","DOIUrl":"10.1107/S205698902500920X","url":null,"abstract":"<div><div>In the title solvates, the indole ring rotations (58–72°) relative to the plane of the central ring govern non-planarity. In the extended structures, N—H⋯O links form chains or sheets and disordered solvents were masked.</div></div><div><div>The syntheses and structures of the dimethyl sulfoxide (DMSO) solvate of 3,6-bis(indol-3-yl)-1,4-dimethylpiperazine-2,5-dione, C<sub>11</sub>H<sub>10</sub>N<sub>2</sub>O (<strong>I</strong>), and of the dimethyl sulfoxide and tetrahydrofuran (THF) solvates of 1,4-dimethyl-3,6-bis(2-methylindol-3-yl)piperazine-2,5-dione, C<sub>12</sub>H<sub>12</sub>N<sub>2</sub>O, (<strong>II</strong>) and (<strong>III</strong>), respectively, are reported. The asymmetric units of (<strong>I</strong>) and (<strong>II</strong>) each contain two crystallographically independent half-molecules that are completed by inversion symmetry, whereas (<strong>III</strong>) contains one independent half-molecule. In all three structures, the piperazine-2,5-dione core is essentially planar and the overall molecular non-planarity arises from rotations of the indole substituents: ranging between 58 and 63° in (<strong>I</strong>), approximately 72° for both independent molecules in (<strong>II</strong>) and approximately 62° in (<strong>III</strong>). In the crystal of (<strong>I</strong>), molecules are linked by two N—H⋯O hydrogen bonds to form <em>C</em>(18) chains; (<strong>II</strong>) features a single N—H⋯O contact giving <em>C</em>(8) chains; and (<strong>III</strong>) exhibits N—H⋯O interactions that generate <em>C</em>(7) chains assembling into sheets lying parallel to (100). No significant π–π stacking is present in any of these structures. All three structures contain regions of disordered solvent (DMSO or THF) that were treated with a solvent mask during refinement.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1071-1075"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480779","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-01DOI: 10.1107/S2056989025009193
Hemant P. Yennawar , Tapas K. Mal , Mark A. Olsen , Anthony F. Lagalante , Aloura D. Gavalis , Isabella G. Frederick , Evelyn M. Louca , Lee J. Silverberg
One of the title compounds shows spontaneous resolution during crystallization.
The title compounds, one a thiazole derivative: (2S)-2-phenyl-3-(thiazol-2-yl)-2,3,5,6-tetrahydro-4H-1,3-thiazin-4-one, C13H12N2OS2, and the second a furan derivative: (rac)-2-(furan-2-yl)-3-phenyl-2,3,5,6-tetrahydro-4H-1,3-thiazin-4-one, C14H13NO2S, crystallize in space-groups P212121 and P21/c, respectively, with a single molecule in their asymmetric units. The crystal of the thiazole derivative chosen for data collection was found to consist of the S enantiomer [Flack parameter 0.013 (9)]. The crystal of the furan derivative in the centrosymmetric space group is a racemic mixture. The puckering of the thiazine ring in both the structures is a half-chair. The extended structure of the thiazole derivative shows two weak C—H⋯O type interactions, but no aromatic ring interactions. In the structure of the furan derivative, an extensive and continuous network of C—H⋯O hydrogen bonds between the furan and the substituted thiazine ring, and also between symmetry-related furan rings, results in a continuous amphiphilic layer lying parallel to the (100) plane. Adjacent to this plane is the layer of hydrophobic phenyl rings. Thus, the extended structure comprises alternating layers of amphiphilic and hydrophobic regions, stacked in the a-axis direction. A C—H⋯O interaction between the phenyl ring and the thiazin-4-one moiety and the π–π stacking of the phenyl rings between pairs of symmetry-related molecules further consolidates the extended structure.
{"title":"Syntheses and structures of spontaneously resolved (2S)-2-phenyl-3-(thiazol-2-yl)-2,3,5,6-tetrahydro-4H-1,3-thiazin-4-one and racemic 2-(furan-2-yl)-3-phenyl-2,3,5,6-tetrahydro-4H-1,3-thiazin-4-one","authors":"Hemant P. Yennawar , Tapas K. Mal , Mark A. Olsen , Anthony F. Lagalante , Aloura D. Gavalis , Isabella G. Frederick , Evelyn M. Louca , Lee J. Silverberg","doi":"10.1107/S2056989025009193","DOIUrl":"10.1107/S2056989025009193","url":null,"abstract":"<div><div>One of the title compounds shows spontaneous resolution during crystallization.</div></div><div><div>The title compounds, one a thiazole derivative: (2<em>S</em>)-2-phenyl-3-(thiazol-2-yl)-2,3,5,6-tetrahydro-4<em>H</em>-1,3-thiazin-4-one, C<sub>13</sub>H<sub>12</sub>N<sub>2</sub>OS<sub>2</sub>, and the second a furan derivative: (<em>rac</em>)-2-(furan-2-yl)-3-phenyl-2,3,5,6-tetrahydro-4<em>H</em>-1,3-thiazin-4-one, C<sub>14</sub>H<sub>13</sub>NO<sub>2</sub>S, crystallize in space-groups <em>P</em>2<sub>1</sub>2<sub>1</sub>2<sub>1</sub> and <em>P</em>2<sub>1</sub>/<em>c</em>, respectively, with a single molecule in their asymmetric units. The crystal of the thiazole derivative chosen for data collection was found to consist of the <em>S</em> enantiomer [Flack parameter 0.013 (9)]. The crystal of the furan derivative in the centrosymmetric space group is a racemic mixture. The puckering of the thiazine ring in both the structures is a half-chair. The extended structure of the thiazole derivative shows two weak C—H⋯O type interactions, but no aromatic ring interactions. In the structure of the furan derivative, an extensive and continuous network of C—H⋯O hydrogen bonds between the furan and the substituted thiazine ring, and also between symmetry-related furan rings, results in a continuous amphiphilic layer lying parallel to the (100) plane. Adjacent to this plane is the layer of hydrophobic phenyl rings. Thus, the extended structure comprises alternating layers of amphiphilic and hydrophobic regions, stacked in the <em>a</em>-axis direction. A C—H⋯O interaction between the phenyl ring and the thiazin-4-one moiety and the π–π stacking of the phenyl rings between pairs of symmetry-related molecules further consolidates the extended structure.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1044-1049"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480304","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-01DOI: 10.1107/S2056989025009119
Julius Hättasch , Annika Schmidt , Carsten Strohmann
The lithium halide dimethyl ether (DME) adducts [Li2Cl2(DME)4] and [Li2Br2(DME)4] form dimeric units linked into layers by CH3⋯Cl tetrel bonds or CH3⋯CH3, CH3⋯O and CH3⋯Br contacts, illustrating the coordination ability of dimethyl ether and its role in directing supramolecular assembly.
Lithium chloride and bromide dimethyl ether adducts, di-μ-chlorido-bis[bis(dimethyl ether-κO)lithium], [Li2Cl2(DME)4] (1), and di-μ-bromido-bis[bis(dimethyl ether-κO)lithium], [Li2Br2(DME)4] (2) [DME is dimethyl ether, C2H6O], have been characterized by single-crystal X-ray diffraction. Both compounds crystallize as dimers, in which the lithium ions are tetrahedrally coordinated by two μ-halide ions and two O-centres from the DME ligands. In 1, the dimers form two-dimensional layers defined by CH3⋯Cl tetrel bonds, while the bromide analogue assembles into planar sheets featuring CH3⋯CH3 contacts. Hirshfeld surface analyses reveal that H⋯H and halogen–hydrogen interactions dominate the intermolecular contacts. The results demonstrate that even the simplest ether, dimethyl ether, can act as an effective coordinating ligand toward lithium halides and influence their aggregation and supramolecular organization. Thereby, this study explores new advances into the preparation and handling of sophisticated coordination compounds with gaseous ligands.
{"title":"Crystal structure and Hirshfeld surface analysis of lithium chloride and lithium bromide with dimethyl ether ligands","authors":"Julius Hättasch , Annika Schmidt , Carsten Strohmann","doi":"10.1107/S2056989025009119","DOIUrl":"10.1107/S2056989025009119","url":null,"abstract":"<div><div>The lithium halide dimethyl ether (DME) adducts [Li<sub>2</sub>Cl<sub>2</sub>(DME)<sub>4</sub>] and [Li<sub>2</sub>Br<sub>2</sub>(DME)<sub>4</sub>] form dimeric units linked into layers by CH<sub>3</sub>⋯Cl tetrel bonds or CH<sub>3</sub>⋯CH<sub>3</sub>, CH<sub>3</sub>⋯O and CH<sub>3</sub>⋯Br contacts, illustrating the coordination ability of dimethyl ether and its role in directing supramolecular assembly.</div></div><div><div>Lithium chloride and bromide dimethyl ether adducts, di-μ-chlorido-bis[bis(dimethyl ether-κ<em>O</em>)lithium], [Li<sub>2</sub>Cl<sub>2</sub>(DME)<sub>4</sub>] (<strong>1</strong>), and di-μ-bromido-bis[bis(dimethyl ether-κ<em>O</em>)lithium], [Li<sub>2</sub>Br<sub>2</sub>(DME)<sub>4</sub>] (<strong>2</strong>) [DME is dimethyl ether, C<sub>2</sub>H<sub>6</sub>O], have been characterized by single-crystal X-ray diffraction. Both compounds crystallize as dimers, in which the lithium ions are tetrahedrally coordinated by two μ-halide ions and two O-centres from the DME ligands. In <strong>1</strong>, the dimers form two-dimensional layers defined by CH<sub>3</sub>⋯Cl tetrel bonds, while the bromide analogue assembles into planar sheets featuring CH<sub>3</sub>⋯CH<sub>3</sub> contacts. Hirshfeld surface analyses reveal that H⋯H and halogen–hydrogen interactions dominate the intermolecular contacts. The results demonstrate that even the simplest ether, dimethyl ether, can act as an effective coordinating ligand toward lithium halides and influence their aggregation and supramolecular organization. Thereby, this study explores new advances into the preparation and handling of sophisticated coordination compounds with gaseous ligands.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1086-1093"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480619","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-01DOI: 10.1107/S2056989025008631
Isha A. Kallingal , Anais A. Alvarado , S. Chantal E. Stieber , Alex John
A μ-oxo vanadium(V) dimeric complex, μ-oxido-bis[(2,2′-{[ethane-1,2-diylbis(azanediyl)]bis(methylene)}diphenolato)oxidovanadium(V)], was synthesized and structurally characterized.
A μ-oxo vanadium(V) dimeric complex, μ-oxido-bis[(2,2′-{[ethane-1,2-diylbis(azanediyl)]bis(methylene)}diphenolato)oxidovanadium(V)],[V2(C16H18N2O2)2O3] (1), was crystallized by slow evaporation from an ethanol solution. The μ-oxo dimer crystallizes in the monoclinic space group C2/c where the salan ligand 1a coordinates to the vanadium center in a κ2N,κ2O fashion, forming a distorted octahedral geometry. The bridging oxo ligand lies on a crystallographic twofold axis. The unit cell consists of four molecules of 1 that are linked by C—H⋯·πarene interactions as well as intramolecular hydrogen bonding.
{"title":"Crystal structure of a μ-oxo vanadium(V) dimer coordinated by a salan ligand","authors":"Isha A. Kallingal , Anais A. Alvarado , S. Chantal E. Stieber , Alex John","doi":"10.1107/S2056989025008631","DOIUrl":"10.1107/S2056989025008631","url":null,"abstract":"<div><div>A <em>μ</em>-oxo vanadium(V) dimeric complex, μ-oxido-bis[(2,2′-{[ethane-1,2-diylbis(azanediyl)]bis(methylene)}diphenolato)oxidovanadium(V)], was synthesized and structurally characterized.</div></div><div><div>A <em>μ</em>-oxo vanadium(V) dimeric complex, μ-oxido-bis[(2,2′-{[ethane-1,2-diylbis(azanediyl)]bis(methylene)}diphenolato)oxidovanadium(V)],[V<sub>2</sub>(C<sub>16</sub>H<sub>18</sub>N<sub>2</sub>O<sub>2</sub>)<sub>2</sub>O<sub>3</sub>] (<strong>1</strong>), was crystallized by slow evaporation from an ethanol solution. The <em>μ</em>-oxo dimer crystallizes in the monoclinic space group <em>C</em>2/<em>c</em> where the salan ligand <strong>1a</strong> coordinates to the vanadium center in a κ<sup>2</sup><em>N</em>,κ<sup>2</sup><em>O</em> fashion, forming a distorted octahedral geometry. The bridging oxo ligand lies on a crystallographic twofold axis. The unit cell consists of four molecules of <strong>1</strong> that are linked by C—H⋯·π<sub>arene</sub> interactions as well as intramolecular hydrogen bonding.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1014-1017"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480674","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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