Pub Date : 2025-11-01DOI: 10.1107/S2056989025008904
Brahim Hni , Ahmed Moussaif , Kostiantyn V. Domasevitch , Joel T. Mague , Ahmed Mazzah , El Mokhtar Essassi , Nada Kheira Sebbar
The crystal structures of two new (Z)-2-arylmethylidene-2H-benzo[b][1,4]thiazin-3(4H)-ones are dominated by mutual hydrogen bonding with the assembly of dimers, which may provide a prototype for reliable supramolecular synthons with the appropriately functionalized substrates for biomedical systems.
Two new 2-arylmethylidene derivatives of benzo-1,4-thiazin-3-one, namely, (Z)-2-(4-methylbenzylidene)-2H-benzo[b][1,4]thiazin-3(4H)-one, C16H13NOS, 1, and (Z)-2-(furan-2-ylmethylidene)-2H-benzo[b][1,4]thiazin-3(4H)-one, C13H9NO2S, 2, are rare examples of a nearly planar structure of the 1,4-thiazin-3-one core stabilized by conjugation. Their supramolecular structures are very similar, being dominated by assembly of inversion dimers through highly directional reciprocal N—H⋯O bonds [N⋯O = 2.822 (2) Å for 1; 2.881 (3) Å for 2]. Weaker forces are represented by C—H⋯O, C—H⋯π and stacking interactions, with more interactions in the case of furfurylidene 2, and they are important for consolidation of the structures. This is consistent with the results of Hirshfeld surface analysis and calculated interaction energies. Doubling the number of O atoms, when moving from 1 to 2, results in even larger increase in fractions of O⋯H/H⋯O contacts [7.6 to 18.6%] due to extensive interactions with the furyl-O acceptor and this contributes to higher packing index in the case of 2. The far superior energetics in the structures are related with the formation of hydrogen-bonded dimers [−73.3 and −72.9 kJ mol−1, for 1 and 2, respectively], followed by dispersion forces and weak C—H⋯O bonding. Identification of reliable 1,4-thiazin-3-one based supramolecular synthons is important for selective targeting for biomedical applications.
苯并-1,4-噻唑-锌-3-酮的两个新的2-芳基甲基二烯衍生物，即(Z)-2-（4-甲基苄基二烯）- 2h -苯并[b][1,4]噻唑-锌-3(4H)-酮，C16H13NOS， 1和(Z)-2-（呋喃-2-基甲基二烯）- 2h -苯并[b][1,4]噻唑-锌-3(4H)-酮，C13H9NO2S, 2，是偶联稳定的1,4-噻唑-锌-3-酮核心的近平面结构的罕见例子。它们的超分子结构非常相似，主要由倒置二聚体通过高度定向的互反N- h⋯O键组装而成[N⋯O = 2.822 (2) Å for 1；2.881 (3) Å for 2]。较弱的力由C-H⋯O， C-H⋯π和堆叠相互作用表示，在糠酰二烯2的情况下，相互作用更多，它们对结构的巩固很重要。这与Hirshfeld表面分析和计算的相互作用能的结果一致。当从1移动到2时，O原子的数量增加一倍，由于与糠基-O受体的广泛相互作用，导致O⋯H/H⋯O接触的分数[7.6至18.6%]增加得更大，这有助于在2的情况下获得更高的堆积指数。这些结构中优异的能量学与氢键二聚体的形成有关[1和2分别为-73.3和-72.9 kJ mol-1]，其次是分散力和弱的C-H⋯O键。鉴定可靠的1,4-硫锌-3-酮基超分子合成子对于生物医学应用的选择性靶向具有重要意义。
{"title":"Crystal structures, Hirshfeld surface analysis and interaction energies of (Z)-2-(4-methylbenzylidene)- and (Z)-2-(furfurylidene)-2H-benzo[b][1,4]thiazin-3(4H)-one","authors":"Brahim Hni , Ahmed Moussaif , Kostiantyn V. Domasevitch , Joel T. Mague , Ahmed Mazzah , El Mokhtar Essassi , Nada Kheira Sebbar","doi":"10.1107/S2056989025008904","DOIUrl":"10.1107/S2056989025008904","url":null,"abstract":"<div><div>The crystal structures of two new (<em>Z</em>)-2-arylmethylidene-2<em>H</em>-benzo[<em>b</em>][1,4]thiazin-3(4<em>H</em>)-ones are dominated by mutual hydrogen bonding with the assembly of dimers, which may provide a prototype for reliable supramolecular synthons with the appropriately functionalized substrates for biomedical systems.</div></div><div><div>Two new 2-arylmethylidene derivatives of benzo-1,4-thiazin-3-one, namely, (<em>Z</em>)-2-(4-methylbenzylidene)-2<em>H</em>-benzo[<em>b</em>][1,4]thiazin-3(4<em>H</em>)-one, C<sub>16</sub>H<sub>13</sub>NOS, <strong>1</strong>, and (<em>Z</em>)-2-(furan-2-ylmethylidene)-2<em>H</em>-benzo[<em>b</em>][1,4]thiazin-3(4<em>H</em>)-one, C<sub>13</sub>H<sub>9</sub>NO<sub>2</sub>S, <strong>2</strong>, are rare examples of a nearly planar structure of the 1,4-thiazin-3-one core stabilized by conjugation. Their supramolecular structures are very similar, being dominated by assembly of inversion dimers through highly directional reciprocal N—H⋯O bonds [N⋯O = 2.822 (2) Å for <strong>1</strong>; 2.881 (3) Å for <strong>2</strong>]. Weaker forces are represented by C—H⋯O, C—H⋯π and stacking interactions, with more interactions in the case of furfurylidene <strong>2</strong>, and they are important for consolidation of the structures. This is consistent with the results of Hirshfeld surface analysis and calculated interaction energies. Doubling the number of O atoms, when moving from <strong>1</strong> to <strong>2</strong>, results in even larger increase in fractions of O⋯H/H⋯O contacts [7.6 to 18.6%] due to extensive interactions with the furyl-O acceptor and this contributes to higher packing index in the case of <strong>2</strong>. The far superior energetics in the structures are related with the formation of hydrogen-bonded dimers [−73.3 and −72.9 kJ mol<sup>−1</sup>, for <strong>1</strong> and <strong>2</strong>, respectively], followed by dispersion forces and weak C—H⋯O bonding. Identification of reliable 1,4-thiazin-3-one based supramolecular synthons is important for selective targeting for biomedical applications.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1055-1062"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480244","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/S2056989025008801
Cindy Döring , Peter G. Jones
<div><div>Packing patterns of the title compounds are analysed in terms of hydrogen bonds, halogen bonds, coinage bonds and halogen⋯π contacts.</div></div><div><div>2-Picolinium tetrachloridoaurate(III), (C<sub>6</sub>H<sub>8</sub>N)[AuCl<sub>4</sub>] or (2-PicH)[AuCl<sub>4</sub>], <strong>1</strong>, and 2-picolinium tetrabromidoaurate(III), (C<sub>6</sub>H<sub>8</sub>N)[AuBr<sub>4</sub>] or (2-PicH)[AuBr<sub>4</sub>], <strong>2</strong>, both crystallize in the space group <em>P</em>1 with <em>Z</em> = 4, but are not isotypic. Bis(2-picolinium) tetrabromidoaurate(III) bromide, (C<sub>6</sub>H<sub>8</sub>N)<sub>2</sub>[AuBr<sub>4</sub>]Br or (2-PicH)<sub>2</sub>[AuBr<sub>4</sub>]Br, <strong>3</strong>, crystallizes in the space group <em>P</em>1 with <em>Z</em> = 2. All atoms of <strong>1</strong>–<strong>3</strong> lie on general positions. 3-Picolinium tetrabromidoaurate(III), (C<sub>6</sub>H<sub>8</sub>N)[AuCl<sub>4</sub>] or (3-PicH)[AuBr<sub>4</sub>], <strong>4</strong>, crystallizes in the space group <em>P</em>2<sub>1</sub>/<em>c</em> with <em>Z</em> = 4; the two independent anions each display inversion symmetry. <em>trans</em>-Dibromidobis(4-picoline)gold(III) tetrabromidoaurate(III) nitromethane monosolvate, [AuBr<sub>2</sub>(C<sub>6</sub>H<sub>7</sub>N)<sub>2</sub>](AuBr<sub>4</sub>]·CH<sub>3</sub>NO<sub>2</sub> or [(4-Pic)<sub>2</sub>AuBr<sub>2</sub>](AuBr<sub>4</sub>]·CH<sub>3</sub>NO<sub>2</sub>, <strong>5</strong>, and 4-picolinium tetrabromidoaurate(III), (C<sub>6</sub>H<sub>8</sub>N)[AuBr<sub>4</sub>] or (4-PicH)[AuBr<sub>4</sub>], <strong>6</strong>, both crystallize in the space group <em>P</em>1 with <em>Z</em> = 2; both involve two independent anions with inversion symmetry. 2,4-Lutidinium tetrabromidoaurate(III), (C<sub>7</sub>H<sub>10</sub>N)[AuBr<sub>4</sub>] or (2,4-LutH)[AuBr<sub>4</sub>], <strong>7</strong>, crystallizes in the space group <em>P</em>2<sub>1</sub>2<sub>1</sub>2<sub>1</sub> with <em>Z</em> = 4. All the gold(III) species show the expected square-planar geometry. The main interest centres on the packing patterns. In <strong>1</strong>, hydrogen bonds, Cl⋯Cl contacts, axial Au⋯Cl contacts (‘coinage bonds’) and Cl⋯π contacts combine to form layers parallel to (101). In <strong>2</strong>, similar contacts (but involving Br) link the residues to form corrugated layers parallel to the <em>ac</em> plane. In <strong>3</strong>, classical hydrogen bonds, Br⋯Br contacts and a coinage bond, all involving the free bromide ion, combine to produce rings of composition Au<sub>2</sub>Br<sub>4</sub>, which are then linked by another Br⋯Br contact, to form chains of residues parallel to [011]. In <strong>4</strong>, hydrogen bonds and a Br⋯Br contact generate chains of residues parallel to [101], which are in turn linked by a Br⋯π contact. In <strong>5</strong>, Br⋯Br contacts and coinage bonds link the anions and cations to form a corrugated layer structure parallel to the <em>ac</em> plane, involvin
{"title":"Crystal structures of trans-dibromidobis(4-picoline)gold(III) tetrabromidoaurate(III) nitromethane monosolvate, bis(2-picolinium) tetrabromidoaurate(III) bromide, and five salts of the type picolinium or lutidinium tetrahalogenidoaurate(III)","authors":"Cindy Döring , Peter G. Jones","doi":"10.1107/S2056989025008801","DOIUrl":"10.1107/S2056989025008801","url":null,"abstract":"<div><div>Packing patterns of the title compounds are analysed in terms of hydrogen bonds, halogen bonds, coinage bonds and halogen⋯π contacts.</div></div><div><div>2-Picolinium tetrachloridoaurate(III), (C<sub>6</sub>H<sub>8</sub>N)[AuCl<sub>4</sub>] or (2-PicH)[AuCl<sub>4</sub>], <strong>1</strong>, and 2-picolinium tetrabromidoaurate(III), (C<sub>6</sub>H<sub>8</sub>N)[AuBr<sub>4</sub>] or (2-PicH)[AuBr<sub>4</sub>], <strong>2</strong>, both crystallize in the space group <em>P</em>1 with <em>Z</em> = 4, but are not isotypic. Bis(2-picolinium) tetrabromidoaurate(III) bromide, (C<sub>6</sub>H<sub>8</sub>N)<sub>2</sub>[AuBr<sub>4</sub>]Br or (2-PicH)<sub>2</sub>[AuBr<sub>4</sub>]Br, <strong>3</strong>, crystallizes in the space group <em>P</em>1 with <em>Z</em> = 2. All atoms of <strong>1</strong>–<strong>3</strong> lie on general positions. 3-Picolinium tetrabromidoaurate(III), (C<sub>6</sub>H<sub>8</sub>N)[AuCl<sub>4</sub>] or (3-PicH)[AuBr<sub>4</sub>], <strong>4</strong>, crystallizes in the space group <em>P</em>2<sub>1</sub>/<em>c</em> with <em>Z</em> = 4; the two independent anions each display inversion symmetry. <em>trans</em>-Dibromidobis(4-picoline)gold(III) tetrabromidoaurate(III) nitromethane monosolvate, [AuBr<sub>2</sub>(C<sub>6</sub>H<sub>7</sub>N)<sub>2</sub>](AuBr<sub>4</sub>]·CH<sub>3</sub>NO<sub>2</sub> or [(4-Pic)<sub>2</sub>AuBr<sub>2</sub>](AuBr<sub>4</sub>]·CH<sub>3</sub>NO<sub>2</sub>, <strong>5</strong>, and 4-picolinium tetrabromidoaurate(III), (C<sub>6</sub>H<sub>8</sub>N)[AuBr<sub>4</sub>] or (4-PicH)[AuBr<sub>4</sub>], <strong>6</strong>, both crystallize in the space group <em>P</em>1 with <em>Z</em> = 2; both involve two independent anions with inversion symmetry. 2,4-Lutidinium tetrabromidoaurate(III), (C<sub>7</sub>H<sub>10</sub>N)[AuBr<sub>4</sub>] or (2,4-LutH)[AuBr<sub>4</sub>], <strong>7</strong>, crystallizes in the space group <em>P</em>2<sub>1</sub>2<sub>1</sub>2<sub>1</sub> with <em>Z</em> = 4. All the gold(III) species show the expected square-planar geometry. The main interest centres on the packing patterns. In <strong>1</strong>, hydrogen bonds, Cl⋯Cl contacts, axial Au⋯Cl contacts (‘coinage bonds’) and Cl⋯π contacts combine to form layers parallel to (101). In <strong>2</strong>, similar contacts (but involving Br) link the residues to form corrugated layers parallel to the <em>ac</em> plane. In <strong>3</strong>, classical hydrogen bonds, Br⋯Br contacts and a coinage bond, all involving the free bromide ion, combine to produce rings of composition Au<sub>2</sub>Br<sub>4</sub>, which are then linked by another Br⋯Br contact, to form chains of residues parallel to [011]. In <strong>4</strong>, hydrogen bonds and a Br⋯Br contact generate chains of residues parallel to [101], which are in turn linked by a Br⋯π contact. In <strong>5</strong>, Br⋯Br contacts and coinage bonds link the anions and cations to form a corrugated layer structure parallel to the <em>ac</em> plane, involvin","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1028-1039"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480715","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/S2056989025008606
Kseniia A. Alekseeva , Atash V. Gurbanov , Mikhail S. Grigoriev , Elena A. Sorokina , Irina A. Kolesnik , Mohammed Hadi Al-Douh , Tuncer Hökelek , Khudayar I. Hasanov
The molecule of the title compound, C16H9BrClNO2, contains furan and phenyl rings and an almost planar isoindole ring system, which is coplanar with the furan ring. In the crystal, C—H⋯O hydrogen bonds link the molecules into a two-dimensional network. π–π stacking helps to consolidate the packing.
The molecule of the title compound, C16H9BrClNO2, contains furan and phenyl rings and an isoindole ring system. The phenyl ring subtends a dihedral angle of 10.3 (2)° with the fused ring system. In the crystal, C—H⋯O hydrogen bonds link the molecules into a two-dimensional network nearly parallel to the ab plane, enclosing R22(6), R44(12), R44(14), R44(18) and R44(20) ring motifs. π–π stacking between the centroids of parallel rings [centroid–centroid distances = 3.919 (3)–3.695 (3) Å] helps to consolidate the packing. Hirshfeld surface analysis revealed that the most important contributions for the crystal packing are from H⋯H (21.2%), H⋯Cl/Cl⋯H (14.7%), H⋯O/O⋯H (13.9%), H⋯C/C⋯H (13.1%), H⋯Br/Br⋯H (12.3%) and C⋯C (11.6%) interactions.
{"title":"Crystal structure and Hirshfeld surface analysis of 4-bromo-6-(4-chlorophenyl)-6,7-dihydro-5H-furo[2,3-f]isoindol-5-one","authors":"Kseniia A. Alekseeva , Atash V. Gurbanov , Mikhail S. Grigoriev , Elena A. Sorokina , Irina A. Kolesnik , Mohammed Hadi Al-Douh , Tuncer Hökelek , Khudayar I. Hasanov","doi":"10.1107/S2056989025008606","DOIUrl":"10.1107/S2056989025008606","url":null,"abstract":"<div><div>The molecule of the title compound, C<sub>16</sub>H<sub>9</sub>BrClNO<sub>2</sub>, contains furan and phenyl rings and an almost planar isoindole ring system, which is coplanar with the furan ring. In the crystal, C—H⋯O hydrogen bonds link the molecules into a two-dimensional network. π–π stacking helps to consolidate the packing.</div></div><div><div>The molecule of the title compound, C<sub>16</sub>H<sub>9</sub>BrClNO<sub>2</sub>, contains furan and phenyl rings and an isoindole ring system. The phenyl ring subtends a dihedral angle of 10.3 (2)° with the fused ring system. In the crystal, C—H⋯O hydrogen bonds link the molecules into a two-dimensional network nearly parallel to the <em>ab</em> plane, enclosing <em>R</em><sup>2</sup><sub>2</sub>(6), <em>R</em><sup>4</sup><sub>4</sub>(12), <em>R</em><sup>4</sup><sub>4</sub>(14), <em>R</em><sup>4</sup><sub>4</sub>(18) and <em>R</em><sup>4</sup><sub>4</sub>(20) ring motifs. π–π stacking between the centroids of parallel rings [centroid–centroid distances = 3.919 (3)–3.695 (3) Å] helps to consolidate the packing. Hirshfeld surface analysis revealed that the most important contributions for the crystal packing are from H⋯H (21.2%), H⋯Cl/Cl⋯H (14.7%), H⋯O/O⋯H (13.9%), H⋯C/C⋯H (13.1%), H⋯Br/Br⋯H (12.3%) and C⋯C (11.6%) interactions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 996-999"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480687","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/S2056989025008722
Tobias Wolflehner , Matthias Weil
The crystal structures of the two title hydrated phases of K3(VO4) consist of isolated vanadate tetrahedra linked via K+ cations. The difference in water content is noticeable in the hydrogen-bonding interactions, which define a finite network for the 0.56-hydrate phase and an infinite network for the 4-hydrate phase.
Single crystals of the hydrated potassium orthovanadate phases K3(VO4)·0.56H2O, tripotassium orthovanadate 0.56-hydrate, and K3(VO4)·4H2O, tripotassium orthovanadate tetrahydrate, were isolated during the processing of products obtained under hydroflux conditions. The asymmetric unit of K3(VO4)(H2O)0.56 (space group P1, Z = 12) comprises six formula units of K3(VO4) and five water molecules of crystallization. The complex crystal structure is made up of isolated [VO4]3– tetrahedra connected via K+ cations exhibiting coordination numbers between 6 and 8. The structure is consolidated by the formation of a finite hydrogen-bonded network between the water molecules and [VO4]3– tetrahedra. Two of the K+ cations are positionally disordered, and three of the water molecules of crystallization are occupationally and/or positionally disordered. The asymmetric unit of K3(VO4)(H2O)4 (space group Pmn21, Z = 2) comprises two K+ cations, one VV atom, three O atoms and two water molecules. The crystal structure is also made up from isolated [VO4]3– tetrahedra interlinked by K+ cations (coordination numbers 7 and 8). In comparison with the less-hydrated phase, the higher water content of this compound results in an infinite network of O—H⋯O hydrogen bonds between the water molecules and [VO4]3– tetrahedra.
在流体通量条件下，分离得到了水合正钒酸钾相K3（VO4）·0.56H2O（0.56-水合物）和K3（VO4）·4H2O（四水合物正钒酸三钾）。K3(VO4)(H2O)0.56（空间群P1， Z = 12）的不对称单元由6个K3（VO4）分子式单元和5个结晶水分子组成。复杂的晶体结构由K+阳离子连接的孤立的[VO4]3-四面体组成，配位数在6到8之间。该结构通过水分子和[VO4]3-四面体之间形成有限氢键网络而巩固。其中两个K+阳离子是位置无序的，三个结晶水分子是位置和/或位置无序的。K3(VO4)(H2O)4（空间群Pmn21， Z = 2）的不对称单元由两个K+阳离子、一个VV原子、三个O原子和两个水分子组成。晶体结构也由K+阳离子（配位数7和8）相互连接的孤立的[VO4]3-四面体组成。与低水合相相比，该化合物的高含水量导致水分子和[VO4]3-四面体之间的O- h⋯O氢键的无限网络。
{"title":"New hydrated phases of potassium orthovanadate: K3(VO4)(H2O)0.56 and K3(VO4)(H2O)4","authors":"Tobias Wolflehner , Matthias Weil","doi":"10.1107/S2056989025008722","DOIUrl":"10.1107/S2056989025008722","url":null,"abstract":"<div><div>The crystal structures of the two title hydrated phases of K<sub>3</sub>(VO<sub>4</sub>) consist of isolated vanadate tetrahedra linked <em>via</em> K<sup>+</sup> cations. The difference in water content is noticeable in the hydrogen-bonding interactions, which define a finite network for the 0.56-hydrate phase and an infinite network for the 4-hydrate phase.</div></div><div><div>Single crystals of the hydrated potassium orthovanadate phases K<sub>3</sub>(VO<sub>4</sub>)·0.56H<sub>2</sub>O, tripotassium orthovanadate 0.56-hydrate, and K<sub>3</sub>(VO<sub>4</sub>)·4H<sub>2</sub>O, tripotassium orthovanadate tetrahydrate, were isolated during the processing of products obtained under hydroflux conditions. The asymmetric unit of K<sub>3</sub>(VO<sub>4</sub>)(H<sub>2</sub>O)<sub>0.56</sub> (space group <em>P</em>1, <em>Z</em> = 12) comprises six formula units of K<sub>3</sub>(VO<sub>4</sub>) and five water molecules of crystallization. The complex crystal structure is made up of isolated [VO<sub>4</sub>]<sup>3–</sup> tetrahedra connected <em>via</em> K<sup>+</sup> cations exhibiting coordination numbers between 6 and 8. The structure is consolidated by the formation of a finite hydrogen-bonded network between the water molecules and [VO<sub>4</sub>]<sup>3–</sup> tetrahedra. Two of the K<sup>+</sup> cations are positionally disordered, and three of the water molecules of crystallization are occupationally and/or positionally disordered. The asymmetric unit of K<sub>3</sub>(VO<sub>4</sub>)(H<sub>2</sub>O)<sub>4</sub> (space group <em>Pmn</em>2<sub>1</sub>, <em>Z</em> = 2) comprises two K<sup>+</sup> cations, one V<sup>V</sup> atom, three O atoms and two water molecules. The crystal structure is also made up from isolated [VO<sub>4</sub>]<sup>3–</sup> tetrahedra interlinked by K<sup>+</sup> cations (coordination numbers 7 and 8). In comparison with the less-hydrated phase, the higher water content of this compound results in an infinite network of O—H⋯O hydrogen bonds between the water molecules and [VO<sub>4</sub>]<sup>3–</sup> tetrahedra.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1008-1013"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480257","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}
The polymorphism of the title salen-type compound synthesized from racemic-(+/-)-1,2-diphenylethylenediamine and 3-chlorosalicylaldehyde is reported
The redetermined structure of a new polymorph of 6,6′-{(1E,1E′)-[(1,2-diphenylethane-1,2-diyl)bis(azaneylylidene)]bis(methaneylylidene)}bis(2-chlorophenol), C28H22Cl2N2O2 was reported. The title compound was synthesized under microwave irradiation at 90 K, within 10 min. The asymmetric unit comprises a potentially tetradentate Schiff base ligand that crystallizes in the triclinic system with space group P1. The structure displays intramolecular O—H⋯N hydrogen bonding, forming an S(6) ring. Comparisons are made with the monoclinic polymorph [Shen et al. (2017). RSC Adv.7, 40640–40649].
报道了6,6′-{（1E,1E′）-[（1,2-二苯基乙烷-1,2-二基）双-（杂氮-内基-二烯）]双-（甲烷-基-二烯）}双-（2-氯酚）C28H22Cl2N2O2的重测定结构。在90 K微波照射下，在10 min内合成了标题化合物。不对称单元包括潜在的四齿状希夫碱配体，该配体在具有空间基团P1的三斜体系中结晶。该结构显示分子内O-H⋯N氢键，形成S(6)环。与单斜晶型进行了比较[Shen et al.(2017)]。中国生物工程学报，2016,36(4):649 - 649。
{"title":"A new triclinic polymorph of 6,6′-{(1E,1E′)-[(1,2-diphenylethane-1,2-diyl)bis(azaneylylidene)]bis(methaneylylidene)}bis(2-chlorophenol)","authors":"Marika Iwatani , Daisuke Nakane , Takashiro Akitsu","doi":"10.1107/S2056989025008850","DOIUrl":"10.1107/S2056989025008850","url":null,"abstract":"<div><div>The polymorphism of the title salen-type compound synthesized from <em>racemic</em>-(+/-)-1,2-diphenylethylenediamine and 3-chlorosalicylaldehyde is reported</div></div><div><div>The redetermined structure of a new polymorph of 6,6′-{(1<em>E</em>,1<em>E</em>′)-[(1,2-diphenylethane-1,2-diyl)bis(azaneylylidene)]bis(methaneylylidene)}bis(2-chlorophenol), C<sub>28</sub>H<sub>22</sub>Cl<sub>2</sub>N<sub>2</sub>O<sub>2</sub> was reported. The title compound was synthesized under microwave irradiation at 90 K, within 10 min. The asymmetric unit comprises a potentially tetradentate Schiff base ligand that crystallizes in the triclinic system with space group <em>P</em>1. The structure displays intramolecular O—H⋯N hydrogen bonding, forming an <em>S</em>(6) ring. Comparisons are made with the monoclinic polymorph [Shen <em>et al.</em> (2017). <em>RSC Adv.</em><strong>7</strong>, 40640–40649].</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1023-1027"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480559","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}
The phenyl ring forms a dihedral angle of 34.72 (6)° with the mean plane of the pyrazolo[3,4-d]pyrimidine ring system.
Heating of 5-amino-1-phenyl-1H-pyrazole-4-carbonitrile in the presence of formic acid yielded the title compound, C11H8N4O. The pyrazolo[3,4-d]pyrimidine ring system forms a dihedral angle of 34.72 (6)° with the phenyl ring. In the crystal, classical N—H⋯O and non-classical C—H⋯O and C—H⋯N intermolecular interactions result in the formation of supramolecular bands extending parallel to the a axis. Additional π⋯π interactions between pyrimidine and pyrazole rings, and C—H⋯π interactions between neighboring phenyl rings consolidate the packing.
{"title":"Crystal structure of 1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one","authors":"Nilufar Akhmedova , Ilkhom Ortikov , Nilufar Khasanova , Kosim Zokhidov , Kambarali Turgunov , Burkhon Elmuradov","doi":"10.1107/S205698902500934X","DOIUrl":"10.1107/S205698902500934X","url":null,"abstract":"<div><div>The phenyl ring forms a dihedral angle of 34.72 (6)° with the mean plane of the pyrazolo[3,4-<em>d</em>]pyrimidine ring system.</div></div><div><div>Heating of 5-amino-1-phenyl-1<em>H</em>-pyrazole-4-carbonitrile in the presence of formic acid yielded the title compound, C<sub>11</sub>H<sub>8</sub>N<sub>4</sub>O. The pyrazolo[3,4-<em>d</em>]pyrimidine ring system forms a dihedral angle of 34.72 (6)° with the phenyl ring. In the crystal, classical N—H⋯O and non-classical C—H⋯O and C—H⋯N intermolecular interactions result in the formation of supramolecular bands extending parallel to the <em>a</em> axis. Additional π⋯π interactions between pyrimidine and pyrazole rings, and C—H⋯π interactions between neighboring phenyl rings consolidate the packing.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1076-1079"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480646","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/S2056989025008618
Evgeniya R. Shelukho , Vladimir P. Zaytsev , Victor N. Khrustalev , Tuncer Hökelek , Khudayar I. Hasanov , Narmina A. Guliyeva , Tahir A. Javadzade , Mohammed Hadi Al-Douh
The molecule of the title compound contains a planar thieno[2,3-f]isoindole ring system and a phenyl ring. In crystal, the molecules are linked through C—H⋯O hydrogen bonds, enclosing R22(14) ring motifs, into a three-dimensional architecture. π–π interactions further consolidate the crystal structure.
In the title compound, C17H11NO3S, the thieno[2,3-f]isoindole ring system and the phenyl ring are oriented at a dihedral angle of 20.57 (13)°. The strong intramolecular O—H⋯O hydrogen bond partly ensures the coplanarity of the carboxyl group and the ring system. In crystal, the molecules are linked through C—H⋯O hydrogen bonds, enclosing R22(14) ring motifs, into a three-dimensional architecture. π–π interactions between parallel five-membered and phenyl rings [centroid-to-centroid distances of 3.564 (3) and 3.591 (3) Å] further contribute to the cohesion of the crystal structure. The Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯H (35.5%), H⋯O/O⋯H (21.3%), C⋯C (14.1%) and H⋯C/C⋯H (12.8%) interactions.
{"title":"Synthesis, crystal structure and Hirshfeld surface analysis of 7-oxo-6-phenyl-6,7-dihydro-5H-thieno[2,3-f]isoindole-8-carboxylic acid","authors":"Evgeniya R. Shelukho , Vladimir P. Zaytsev , Victor N. Khrustalev , Tuncer Hökelek , Khudayar I. Hasanov , Narmina A. Guliyeva , Tahir A. Javadzade , Mohammed Hadi Al-Douh","doi":"10.1107/S2056989025008618","DOIUrl":"10.1107/S2056989025008618","url":null,"abstract":"<div><div>The molecule of the title compound contains a planar thieno[2,3-<em>f</em>]isoindole ring system and a phenyl ring. In crystal, the molecules are linked through C—H⋯O hydrogen bonds, enclosing <em>R</em><sup>2</sup><sub>2</sub>(14) ring motifs, into a three-dimensional architecture. π–π interactions further consolidate the crystal structure.</div></div><div><div>In the title compound, C<sub>17</sub>H<sub>11</sub>NO<sub>3</sub>S, the thieno[2,3-<em>f</em>]isoindole ring system and the phenyl ring are oriented at a dihedral angle of 20.57 (13)°. The strong intramolecular O—H⋯O hydrogen bond partly ensures the coplanarity of the carboxyl group and the ring system. In crystal, the molecules are linked through C—H⋯O hydrogen bonds, enclosing <em>R</em><sup>2</sup><sub>2</sub>(14) ring motifs, into a three-dimensional architecture. π–π interactions between parallel five-membered and phenyl rings [centroid-to-centroid distances of 3.564 (3) and 3.591 (3) Å] further contribute to the cohesion of the crystal structure. The Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯H (35.5%), H⋯O/O⋯H (21.3%), C⋯C (14.1%) and H⋯C/C⋯H (12.8%) interactions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1000-1003"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480566","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}
The title compound is a multi-substituted piperidine derivative in which the piperidine ring adopts a chair conformation.
The title compound, C29H31NO2, is a multi-substituted piperidine derivative in which the piperidine ring adopts a chair conformation. Intermolecular C—H⋯O hydrogen bonds as well as C—H⋯π interactions are observed in the crystal, leading to the formation of inversion dimers and chains, respectively. The intermolecular interactions were quantified and analysed using Hirshfeld surface analysis, revealing that H⋯H interactions contribute the most (70.5%) to the crystal packing.
{"title":"Crystal structure and Hirshfeld surface analysis of 1,3,3-trimethyl-2,6-diphenylpiperidin-4-yl 2-phenylprop-2-enoate","authors":"Aranganathan Ananthabharathi , Sekar Janarthanan , Mannathusamy Gopalakrishnan , Srinivasan Pazhamalai , Sivashanmugam Selvanayagam","doi":"10.1107/S2056989025008709","DOIUrl":"10.1107/S2056989025008709","url":null,"abstract":"<div><div>The title compound is a multi-substituted piperidine derivative in which the piperidine ring adopts a chair conformation.</div></div><div><div>The title compound, C<sub>29</sub>H<sub>31</sub>NO<sub>2</sub>, is a multi-substituted piperidine derivative in which the piperidine ring adopts a chair conformation. Intermolecular C—H⋯O hydrogen bonds as well as C—H⋯π interactions are observed in the crystal, leading to the formation of inversion dimers and chains, respectively. The intermolecular interactions were quantified and analysed using Hirshfeld surface analysis, revealing that H⋯H interactions contribute the most (70.5%) to the crystal packing.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1004-1007"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480552","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/S2056989025008886
Anna Ben , Lilianna Chęcińska
The crystal structure of a new orthorhombic polymorph of pure isavuconazole has been determined and and is compared with the known monoclinic form.
The title compound C22H17F2N5OS (systematic name: 4-{2-[(2R,3R)-3-(2,5-difluorophenyl)-3-hydroxy-4-(1,2,4-triazol-1-yl)butan-2-yl]-1,3-thiazol-4-yl}benzonitrile), represents a new orthorhombic polymorph of isavuconazole. The two stereogenic centers adopt the R,R configuration. In the crystal structure of the orthorhombic form, a mono-periodic chain motif is formed by a strong O—H⋯N hydrogen bond, while three additional C—H⋯N interactions propagate these chains into a tri-periodic supramolecular network. A comparison with the previously reported monoclinic polymorph [Voronin et al. (2021#). CrystEngComm23, 8513] is provided, supported by Hirshfeld surface and energy framework analyses.
标题化合物C22H17F2N5OS(系统名称：4-{2-[（2R,3R)-3-（2,5-二氟苯基）-3-羟基-4-（1,2,4-三唑-1-基）丁-2-基]-1,3-噻唑-4-基}苯腈）是异戊康唑的一种新的邻菱型多晶化合物。两个立体中心采用R，R构型。在正交方阵形式的晶体结构中，单周期链基序由强O-H⋯N氢键形成，而三个额外的C-H⋯N相互作用将这些链传播成三周期超分子网络。与先前报道的单斜晶型的比较[Voronin et al.（2021▸）]。在Hirshfeld表面和能量框架分析的支持下，提供了CrystEngComm 23, 8513]。
{"title":"An orthorhombic polymorph of isavuconazole","authors":"Anna Ben , Lilianna Chęcińska","doi":"10.1107/S2056989025008886","DOIUrl":"10.1107/S2056989025008886","url":null,"abstract":"<div><div>The crystal structure of a new orthorhombic polymorph of pure isavuconazole has been determined and and is compared with the known monoclinic form.</div></div><div><div>The title compound C<sub>22</sub>H<sub>17</sub>F<sub>2</sub>N<sub>5</sub>OS (systematic name: 4-{2-[(2<em>R</em>,3<em>R</em>)-3-(2,5-difluorophenyl)-3-hydroxy-4-(1,2,4-triazol-1-yl)butan-2-yl]-1,3-thiazol-4-yl}benzonitrile), represents a new orthorhombic polymorph of isavuconazole. The two stereogenic centers adopt the <em>R</em>,<em>R</em> configuration. In the crystal structure of the orthorhombic form, a mono-periodic chain motif is formed by a strong O—H⋯N hydrogen bond, while three additional C—H⋯N interactions propagate these chains into a tri-periodic supramolecular network. A comparison with the previously reported monoclinic polymorph [Voronin <em>et al.</em> (2021<span><span>#</span></span>). <em>CrystEngComm</em><strong>23</strong>, 8513] is provided, supported by Hirshfeld surface and energy framework analyses.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1018-1022"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480606","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}
The two compounds Ag3ISO4 and Ag4I2SO4, comprising Ag and I atoms and SO4 tetrahedra, exhibit characteristic silver arrangements, with Ag3ISO4 containing triangularly arranged Ag atoms in zigzag ladder chains along the a-axis direction and Ag4I2SO4 featuring discrete Ag4 clusters.
The crystal structures of two phases in the AgI–Ag2SO4 system, Ag3ISO4(AgI:Ag2SO4 = 1:1; systematic name: trisilver iodide sulfate), and Ag4I2SO4 (AgI:Ag2SO4 = 2:1; systematic name: tetrasilver diiodide sulfate), were determined by single-crystal X-ray diffraction. The crystal structure model of Ag3ISO4 contains triangularly arranged Ag atoms in zigzag ladder chains extending parallel to the a axis. The Ag zigzag ladder chains alternate with rows of SO4 groups, while iodine atoms are accommodated within the concavities of the zigzag ladders. The crystal structure of Ag4I2SO4 was refined using a split-atom model for two of the four Ag sites. The disordered Ag sites are situated between the layers containing SO4 groups parallel to the ac plane, whereas the Ag sites within the SO4 layers are fully occupied and exhibit no disorder. The positional disorder of some of the Ag sites is considered to be associated with the moderate ionic conductivity of Ag4I2SO4, approximately 10−3 S cm−1 at room temperature. This is the first report describing the crystal structures of compounds containing Ag+, SO42– and I−.
采用单晶x射线衍射法测定了Ag3ISO4（AgI:Ag2SO4 = 1:1，学名：三碘化银硫酸酯）和Ag4I2SO4 （AgI:Ag2SO4 = 2:1，学名：四碘化银硫酸酯）两相Ag3ISO4 -Ag2SO4体系的晶体结构。Ag3ISO4的晶体结构模型包含三角形排列的银原子，呈锯齿状阶梯链，平行于a轴延伸。Ag之字形阶梯链与一排排SO4基团交替排列，而碘原子则被安置在锯齿状阶梯的凹槽内。采用原子分裂模型对四个Ag位中的两个进行了细化。无序的Ag位位于与ac平面平行的含有SO4基团的层之间，而SO4层内的Ag位被完全占据，没有表现出无序。一些Ag位的位置紊乱被认为与Ag4I2SO4的中等离子电导率有关，在室温下约为10-3 S cm-1。本文首次报道了含Ag+、so2 -和I-化合物的晶体结构。
{"title":"Crystal structures of the silver iodide sulfates Ag3ISO4 and Ag4I2SO4","authors":"Yuta Matsushima , Kento Uchida , Ryota Kawanago , Mizuki Yamamoto , Hisanori Yamane","doi":"10.1107/S2056989025008898","DOIUrl":"10.1107/S2056989025008898","url":null,"abstract":"<div><div>The two compounds Ag<sub>3</sub>ISO<sub>4</sub> and Ag<sub>4</sub>I<sub>2</sub>SO<sub>4</sub>, comprising Ag and I atoms and SO<sub>4</sub> tetrahedra, exhibit characteristic silver arrangements, with Ag<sub>3</sub>ISO<sub>4</sub> containing triangularly arranged Ag atoms in zigzag ladder chains along the <em>a-</em>axis direction and Ag<sub>4</sub>I<sub>2</sub>SO<sub>4</sub> featuring discrete Ag<sub>4</sub> clusters.</div></div><div><div>The crystal structures of two phases in the AgI–Ag<sub>2</sub>SO<sub>4</sub> system, Ag<sub>3</sub>ISO<sub>4</sub>(AgI:Ag<sub>2</sub>SO<sub>4</sub> = 1:1; systematic name: trisilver iodide sulfate), and Ag<sub>4</sub>I<sub>2</sub>SO<sub>4</sub> (AgI:Ag<sub>2</sub>SO<sub>4</sub> = 2:1; systematic name: tetrasilver diiodide sulfate), were determined by single-crystal X-ray diffraction. The crystal structure model of Ag<sub>3</sub>ISO<sub>4</sub> contains triangularly arranged Ag atoms in zigzag ladder chains extending parallel to the <em>a</em> axis. The Ag zigzag ladder chains alternate with rows of SO<sub>4</sub> groups, while iodine atoms are accommodated within the concavities of the zigzag ladders. The crystal structure of Ag<sub>4</sub>I<sub>2</sub>SO<sub>4</sub> was refined using a split-atom model for two of the four Ag sites. The disordered Ag sites are situated between the layers containing SO<sub>4</sub> groups parallel to the <em>ac</em> plane, whereas the Ag sites within the SO<sub>4</sub> layers are fully occupied and exhibit no disorder. The positional disorder of some of the Ag sites is considered to be associated with the moderate ionic conductivity of Ag<sub>4</sub>I<sub>2</sub>SO<sub>4</sub>, approximately 10<sup>−3</sup> S cm<sup>−1</sup> at room temperature. This is the first report describing the crystal structures of compounds containing Ag<sup>+</sup>, SO<sub>4</sub><sup>2–</sup> and I<sup>−</sup>.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1080-1085"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480776","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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