Pub Date : 2025-11-01DOI: 10.1107/S2056989025009284
Atash V. Gurbanov , Mehmet Akkurt , Nurlana D. Sadikhova , Gizachew Mulugeta Manahelohe
In the crystal, the molecules are linked into [010] chains by C—H⋯O hydrogen bonds, creating a C(6) motif. Weak C—H⋯Cl and C—H⋯F interactions link these chains, forming sheets parallel to the (100) plane.
In the title compound, C19H14ClFO2S2, the molecular conformation is stabilized by intramolecular C—H⋯F, C—H⋯Cl and C—H⋯O hydrogen bonds. In the crystal, the molecules are linked into [010] chains by C—H⋯O hydrogen bonds, creating a C(6) motif and weak C—H⋯F and C—H⋯Cl interactions link these chains into sheets parallel to the (100) plane. The entire –C6H3FCl group is disordered over two positions in a 0.931 (4):0.069 (4) ratio. A Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (26.7%), C⋯H/H⋯C (17.2%), S⋯H/H⋯S (15.0%) and O⋯H/H⋯O (12.0%) interactions.
{"title":"Crystal structure and Hirshfeld surface analysis of 3-(2-chloro-6-fluorophenyl)-1,5-bis(thiophen-2-yl)pentane-1,5-dione","authors":"Atash V. Gurbanov , Mehmet Akkurt , Nurlana D. Sadikhova , Gizachew Mulugeta Manahelohe","doi":"10.1107/S2056989025009284","DOIUrl":"10.1107/S2056989025009284","url":null,"abstract":"<div><div>In the crystal, the molecules are linked into [010] chains by C—H⋯O hydrogen bonds, creating a <em>C</em>(6) motif. Weak C—H⋯Cl and C—H⋯F interactions link these chains, forming sheets parallel to the (100) plane.</div></div><div><div>In the title compound, C<sub>19</sub>H<sub>14</sub>ClFO<sub>2</sub>S<sub>2</sub>, the molecular conformation is stabilized by intramolecular C—H⋯F, C—H⋯Cl and C—H⋯O hydrogen bonds. In the crystal, the molecules are linked into [010] chains by C—H⋯O hydrogen bonds, creating a <em>C</em>(6) motif and weak C—H⋯F and C—H⋯Cl interactions link these chains into sheets parallel to the (100) plane. The entire –C<sub>6</sub>H<sub>3</sub>FCl group is disordered over two positions in a 0.931 (4):0.069 (4) ratio. A Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (26.7%), C⋯H/H⋯C (17.2%), S⋯H/H⋯S (15.0%) and O⋯H/H⋯O (12.0%) interactions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1094-1098"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480665","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/S2056989025008655
Illia Terpeliuk , Kateryna Znovjyak , Sergiu Shova , Olexandr V. Oksiuta , Vladimir M. Amirkhanov , Igor O. Fritsky , Maksym Seredyuk
The title compound, [Fe(C18H11N6O)2]·2CH3OH, crystallizes in the orthorhombic space group, with a distorted pseudooctahedral FeII coordination sphere formed by two deprotonated tridentate 3-(benzofuran-6-yl)-5-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-4H-1,2,4-triazol ligands. In the crystal, molecules stack in chains along the b-axis direction connected by weak C—H(pz)⋯π(ph) interactions and linked into layers by C—H⋯N/C/O interactions, which were quantified by Hirshfeld surface and energy framework analysis.
The title compound, [Fe(C18H11N6O)2]·2CH3OH, crystallizes in the orthorhombic space group Pbcn (No. 60) with half of the complex molecule and a methanol molecule in the asymmetric unit. In the complex, the two tridentate 3-(benzofuran-6-yl)-5-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-4H-1,2,4-triazol ligands meridionally bind to the central FeII ion through the N atoms of the heterocyclic groups, forming a pseudo-octahedral coordination sphere. In the crystal, C—H(pz)⋯π(ph) and C—H⋯N/C/O interactions consolidate the structure. Energy framework analysis at the B3LYP/6–31 G(d,p) theory level was performed to quantify the interaction energies in the crystal.
标题化合物[Fe(C18H11N6O)2]·2CH3OH在邻方阵空间基Pbcn （No. 60）中结晶，其中一半的配合物分子和一个甲醇分子在不对称单元中结晶。在配合物中，两个三齿体3-（苯并呋喃-6-基）-5-[6-（1h -吡唑-1-基）吡啶-2-基]- 4h -1,2,4-三唑配体经向通过杂环基团的N原子与中心FeII离子结合，形成伪八面体配位球。在晶体中，C- h (pz)⋯π(ph)和C- h⋯N/C/O相互作用巩固了结构。在B3LYP/6-31 G（d,p）理论水平上进行能量框架分析，量化晶体中的相互作用能。
{"title":"Crystal structure, Hirshfeld surface and energy framework analysis of bis{3-(benzofuran-6-yl)-5-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-1H-1,2,4-triazol-1-ido}iron(II) methanol disolvate","authors":"Illia Terpeliuk , Kateryna Znovjyak , Sergiu Shova , Olexandr V. Oksiuta , Vladimir M. Amirkhanov , Igor O. Fritsky , Maksym Seredyuk","doi":"10.1107/S2056989025008655","DOIUrl":"10.1107/S2056989025008655","url":null,"abstract":"<div><div>The title compound, [Fe(C<sub>18</sub>H<sub>11</sub>N<sub>6</sub>O)<sub>2</sub>]·2CH<sub>3</sub>OH, crystallizes in the orthorhombic space group, with a distorted pseudooctahedral Fe<sup>II</sup> coordination sphere formed by two deprotonated tridentate 3-(benzofuran-6-yl)-5-[6-(1<em>H</em>-pyrazol-1-yl)pyridin-2-yl]-4<em>H</em>-1,2,4-triazol ligands. In the crystal, molecules stack in chains along the <em>b</em>-axis direction connected by weak C—H(pz)⋯π(ph) interactions and linked into layers by C—H⋯N/C/O interactions, which were quantified by Hirshfeld surface and energy framework analysis.</div></div><div><div>The title compound, [Fe(C<sub>18</sub>H<sub>11</sub>N<sub>6</sub>O)<sub>2</sub>]·2CH<sub>3</sub>OH, crystallizes in the orthorhombic space group <em>Pbcn</em> (No. 60) with half of the complex molecule and a methanol molecule in the asymmetric unit. In the complex, the two tridentate 3-(benzofuran-6-yl)-5-[6-(1<em>H</em>-pyrazol-1-yl)pyridin-2-yl]-4<em>H</em>-1,2,4-triazol ligands meridionally bind to the central Fe<sup>II</sup> ion through the N atoms of the heterocyclic groups, forming a pseudo-octahedral coordination sphere. In the crystal, C—H(pz)⋯π(ph) and C—H⋯N/C/O interactions consolidate the structure. Energy framework analysis at the B3LYP/6–31 G(d,p) theory level was performed to quantify the interaction energies in the crystal.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 991-995"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480753","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/S2056989025009065
Dmytro A. Haleliuk , Laurentiu Baltag , Dina D. Naumova , Valeriia O. Zozulia , Sofiia V. Partsevska
The crystal structure of (C6H14N2)[Br3]2 contains diprotonated triethylenediaminium cations, the charge of which is compensated by [Br3]− anions. The crystal packing is stabilized by Br⋯Br contacts, forming two-dimensional layers, and by N—H⋯Br/C—H⋯Br interactions between cations and tribromide anions.
The crystal structure of the title salt, 1,4-diazabicyclo[2.2.2]octanediium bis(tribromide), (C6H14N2)[Br3]2, consists of diprotonated 1,4-diazabicyclo[2.2.2]octanediium (or triethylenediamine) cations, which are separated by [Br3]− anions. Br⋯Br contacts between polybromide anions generate supramolecular two-dimensional layers propagating along the bc plane. Organic cations are accommodated inside anionic layers and interact with tribromide anions through N—H⋯Br contacts. The structure is additionally stabilized by weak C—H⋯Br interactions linking the organic cations and [Br3]−. Hirshfeld surface analysis and associated fingerprint plots reveal that the main contributions to the crystal packing are provided by Br⋯H interactions (84.8%), followed by less chemically meaningful H⋯H (15.2%) contacts. As a novel example of a tribromide salt, the reported compound is of interest toward its potential use in organic synthesis as a regioselective brominating agent, in oxidation chemistry, and in materials processing involving metal dissolution and recovery.
{"title":"Crystal structure and Hirshfeld surface analysis of 1,4-diazabicyclo[2.2.2]octanediium bis(tribromide)","authors":"Dmytro A. Haleliuk , Laurentiu Baltag , Dina D. Naumova , Valeriia O. Zozulia , Sofiia V. Partsevska","doi":"10.1107/S2056989025009065","DOIUrl":"10.1107/S2056989025009065","url":null,"abstract":"<div><div>The crystal structure of (C<sub>6</sub>H<sub>14</sub>N<sub>2</sub>)[Br<sub>3</sub>]<sub>2</sub> contains diprotonated triethylenediaminium cations, the charge of which is compensated by [Br<sub>3</sub>]<sup>−</sup> anions. The crystal packing is stabilized by Br⋯Br contacts, forming two-dimensional layers, and by N—H⋯Br/C—H⋯Br interactions between cations and tribromide anions.</div></div><div><div>The crystal structure of the title salt, 1,4-diazabicyclo[2.2.2]octanediium bis(tribromide), (C<sub>6</sub>H<sub>14</sub>N<sub>2</sub>)[Br<sub>3</sub>]<sub>2</sub>, consists of diprotonated 1,4-diazabicyclo[2.2.2]octanediium (or triethylenediamine) cations, which are separated by [Br<sub>3</sub>]<sup>−</sup> anions. Br⋯Br contacts between polybromide anions generate supramolecular two-dimensional layers propagating along the <em>bc</em> plane. Organic cations are accommodated inside anionic layers and interact with tribromide anions through N—H⋯Br contacts. The structure is additionally stabilized by weak C—H⋯Br interactions linking the organic cations and [Br<sub>3</sub>]<sup>−</sup>. Hirshfeld surface analysis and associated fingerprint plots reveal that the main contributions to the crystal packing are provided by Br⋯H interactions (84.8%), followed by less chemically meaningful H⋯H (15.2%) contacts. As a novel example of a tribromide salt, the reported compound is of interest toward its potential use in organic synthesis as a regioselective brominating agent, in oxidation chemistry, and in materials processing involving metal dissolution and recovery.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 11","pages":"Pages 1067-1070"},"PeriodicalIF":0.6,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145480517","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 crystal structure of the cobalt complex [Co(C5H7O2)2(C7H6N2S)(H2O)] was determined in the triclinic space group Pī. The unit cell consists of two independent complex molecules linked by N—H⋯O and O—H⋯O hydrogen bonds along the [011] direction. Hirshfeld surface analysis revealed that the largest contributions to the crystal packing originate from H⋯H, H⋯C/C⋯H, O⋯H/H⋯O, and H⋯S/S⋯H contacts.
The crystal structure of the title complex, [Co(C5H7O2)2(C7H6N2S)(H2O)], was determined in the triclinic space group P1. The central CoII ion adopts a slightly distorted octahedral geometry. The unit cell consists of two complex molecules connected via N—H⋯O and O—H⋯O hydrogen bonds along the [011] direction. Hirshfeld surface analysis revealed that the largest contributions to the crystal packing originate from H⋯H (51.8%), H⋯C/C⋯H (16.6%), O⋯H/H⋯O (12.4%), and H⋯S/S⋯H (8.8%) contacts.
{"title":"Synthesis, crystal structure and Hirshfeld surface analysis of (2-aminobenzothiazole-κN3)aquabis(4-oxopent-2-en-2-olato-κ2O,O′)cobalt(II)","authors":"Iroda Tojiboyeva , Sardor Murodov , Lola Makhmudova , Daminbek Ziyatov , Jamshid Ashurov , Shakhlo Daminova","doi":"10.1107/S2056989025008011","DOIUrl":"10.1107/S2056989025008011","url":null,"abstract":"<div><div>The crystal structure of the cobalt complex [Co(C<sub>5</sub>H<sub>7</sub>O<sub>2</sub>)<sub>2</sub>(C<sub>7</sub>H<sub>6</sub>N<sub>2</sub>S)(H<sub>2</sub>O)] was determined in the triclinic space group <em>P</em>ī. The unit cell consists of two independent complex molecules linked by N—H⋯O and O—H⋯O hydrogen bonds along the [011] direction. Hirshfeld surface analysis revealed that the largest contributions to the crystal packing originate from H⋯H, H⋯C/C⋯H, O⋯H/H⋯O, and H⋯S/S⋯H contacts.</div></div><div><div>The crystal structure of the title complex, [Co(C<sub>5</sub>H<sub>7</sub>O<sub>2</sub>)<sub>2</sub>(C<sub>7</sub>H<sub>6</sub>N<sub>2</sub>S)(H<sub>2</sub>O)], was determined in the triclinic space group <em>P</em>1. The central Co<sup>II</sup> ion adopts a slightly distorted octahedral geometry. The unit cell consists of two complex molecules connected <em>via</em> N—H⋯O and O—H⋯O hydrogen bonds along the [011] direction. Hirshfeld surface analysis revealed that the largest contributions to the crystal packing originate from H⋯H (51.8%), H⋯C/C⋯H (16.6%), O⋯H/H⋯O (12.4%), and H⋯S/S⋯H (8.8%) contacts.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 10","pages":"Pages 948-953"},"PeriodicalIF":0.6,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243460","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 : 2025-10-01DOI: 10.1107/S2056989025008084
Chaluvarangaiah Sowbhagya , Thaluru M. Mohan Kumar , Papegowda Bhavya , Hemmige S. Yathirajan , Sean Parkin
The crystal structure and Hirshfeld surface analysis of N-[1-(4-tert-butyl-2-ethoxyphenyl)-2-hydroxyethyl]-2,6-difluorobenzamide, C21H25F2NO3, a metabolite of the insecticide/acaricide etoxazole designated R4, is presented.
A metabolite of the insecticide/acaricide etoxazole, designated R4 {systematic name N-[1-(4-tert-butyl-2-ethoxyphenyl)-2-hydroxyethyl]-2,6-difluorobenzamide, C21H25F2NO3}, is presented. The molecular structure has a central N-(2-hydroxyethyl)formamide group flanked by 4-tert-butyl-2-ethoxyphenyl and 2,6-difluorophenyl-substituted rings. The overall conformation is defined by its torsional degrees of freedom [N—C—C—C = 56.09 (18) and 99.41 (18)°], which place the 4-tert-butyl-2-ethoxyphenyl and 2,6-difluorophenyl rings at a dihedral angle of 70.66 (5)°. In the crystal, molecules are linked by a strong O—H—O hydrogen bond into chains that extend parallel to the a-axis. There are also weaker C—H—F and π-stacking [centroid–centroid distance = 4.266 (2) Å] interactions. A Hirshfeld surface analysis reveals that the intermolecular contacts are dominated by interactions involving hydrogen, the most abundant being H⋯H (54.1%), H⋯O/O⋯H (13.0%), H⋯F/F⋯H (12.8%), and H⋯C/C⋯H (12.8%).
{"title":"Crystal structure and Hirshfeld surface analysis of an etoxazole metabolite designated R4","authors":"Chaluvarangaiah Sowbhagya , Thaluru M. Mohan Kumar , Papegowda Bhavya , Hemmige S. Yathirajan , Sean Parkin","doi":"10.1107/S2056989025008084","DOIUrl":"10.1107/S2056989025008084","url":null,"abstract":"<div><div>The crystal structure and Hirshfeld surface analysis of <em>N</em>-[1-(4-<em>tert</em>-butyl-2-ethoxyphenyl)-2-hydroxyethyl]-2,6-difluorobenzamide, C<sub>21</sub>H<sub>25</sub>F<sub>2</sub>NO<sub>3</sub>, a metabolite of the insecticide/acaricide etoxazole designated <strong>R4</strong>, is presented.</div></div><div><div>A metabolite of the insecticide/acaricide etoxazole, designated <strong>R4</strong> {systematic name <em>N</em>-[1-(4-<em>tert</em>-butyl-2-ethoxyphenyl)-2-hydroxyethyl]-2,6-difluorobenzamide, C<sub>21</sub>H<sub>25</sub>F<sub>2</sub>NO<sub>3</sub>}, is presented. The molecular structure has a central <em>N</em>-(2-hydroxyethyl)formamide group flanked by 4-<em>tert</em>-butyl-2-ethoxyphenyl and 2,6-difluorophenyl-substituted rings. The overall conformation is defined by its torsional degrees of freedom [N—C—C—C = 56.09 (18) and 99.41 (18)°], which place the 4-<em>tert</em>-butyl-2-ethoxyphenyl and 2,6-difluorophenyl rings at a dihedral angle of 70.66 (5)°. In the crystal, molecules are linked by a strong O—H—O hydrogen bond into chains that extend parallel to the <em>a</em>-axis. There are also weaker C—H—F and π-stacking [centroid–centroid distance = 4.266 (2) Å] interactions. A Hirshfeld surface analysis reveals that the intermolecular contacts are dominated by interactions involving hydrogen, the most abundant being H⋯H (54.1%), H⋯O/O⋯H (13.0%), H⋯F/F⋯H (12.8%), and H⋯C/C⋯H (12.8%).</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 10","pages":"Pages 964-967"},"PeriodicalIF":0.6,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243619","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 : 2025-10-01DOI: 10.1107/S2056989025003317
M. Harish Kumar , S. Santhosh Kumar , H. C. Devarajegowda , H. T. Srinivasa , B. S. Palakshamurthy
In the title compound, the aromatic rings are oriented at a dihedral angle of 83.30 (2)°. An intramolecular C—H⋯O contact generates a five-membered S(5) ring motif. In the crystal, C—H⋯O hydrogen bonds link the molecules through R12(6), R22(10), R22(14) hydrogen-bond motifs.
The asymmetric unit of the compound C20H20BrClO3 contains one independent molecule in which the aromatic rings are oriented at a dihedral angle of 83.30 (2)°. An intramolecular C—H⋯O contact generates a five-membered S(5) ring motif. In the crystal, C—H⋯O hydrogen bonds link the molecules through R12(6), R22(10), R22(14) hydrogen-bond motifs. The structure is consolidated by C—H⋯π interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (32.8%), C⋯H/H⋯C (28.1%), O⋯H/H⋯O (14.0%) Br⋯H/H⋯Br (12.5%) and Cl⋯H/H⋯Cl (10.6%) interactions.
{"title":"Crystal structure and Hirshfeld surface studies of 4-bromo-2-chlorophenyl (2E)-3-[4-(pentyloxy)phenyl]prop-2-enoate","authors":"M. Harish Kumar , S. Santhosh Kumar , H. C. Devarajegowda , H. T. Srinivasa , B. S. Palakshamurthy","doi":"10.1107/S2056989025003317","DOIUrl":"10.1107/S2056989025003317","url":null,"abstract":"<div><div>In the title compound, the aromatic rings are oriented at a dihedral angle of 83.30 (2)°. An intramolecular C—H⋯O contact generates a five-membered <em>S</em>(5) ring motif. In the crystal, C—H⋯O hydrogen bonds link the molecules through <em>R</em><sup>1</sup><sub>2</sub>(6), <em>R</em><sup>2</sup><sub>2</sub>(10), <em>R</em><sup>2</sup><sub>2</sub>(14) hydrogen-bond motifs.</div></div><div><div>The asymmetric unit of the compound C<sub>20</sub>H<sub>20</sub>BrClO<sub>3</sub> contains one independent molecule in which the aromatic rings are oriented at a dihedral angle of 83.30 (2)°. An intramolecular C—H⋯O contact generates a five-membered <em>S</em>(5) ring motif. In the crystal, C—H⋯O hydrogen bonds link the molecules through <em>R</em><sup>1</sup><sub>2</sub>(6), <em>R</em><sup>2</sup><sub>2</sub>(10), <em>R</em><sup>2</sup><sub>2</sub>(14) hydrogen-bond motifs. The structure is consolidated by C—H⋯π interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (32.8%), C⋯H/H⋯C (28.1%), O⋯H/H⋯O (14.0%) Br⋯H/H⋯Br (12.5%) and Cl⋯H/H⋯Cl (10.6%) interactions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 10","pages":"Pages 912-915"},"PeriodicalIF":0.6,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243644","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 : 2025-10-01DOI: 10.1107/S2056989025007467
Kateryna Znovjyak , Sergiu Shova , Sergiy O. Nikitin , Yurii S. Moroz , Oksana Tananaiko , Sergey O. Malinkin , Maksym Seredyuk
The title compound, a neutral bis{3-(4-bromophenyl)-5-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-4H-1,2,4-triazol-4-ido}nickel(II) methanol disolvate, exhibits a distorted pseudooctahedral coordination environment around the metal ion. Due to the conical geometry and polar characteristics the molecules stack in one-dimensional columns that are connected by weak hydrogen bonds to form layers. These layers are arranged in a three-dimensional lattice without interlayer interactions closer than van der Waals distances.
The unit cell of the title compound, [Ni(C16H10BrN6)2]·2CH3OH, contains a neutral complex and two methanol molecules. The NiII ion adopts a pseudooctahedral geometry, coordinated by two tridentate ligands via pyrazole, pyridine, and triazole N atoms. The average Ni—N bond length is 2.097 (4) Å. In the crystal, molecules form supramolecular chains through weak C–H⋯π interactions and further assemble into diperiodic layers via C—H⋯N/C interactions. Hirshfeld surface analysis shows H⋯H (32.1%), H⋯C/C⋯H (27.3%), H⋯N/N⋯H (14.9%), and H⋯Br/Br⋯H (14.6%) contacts. Interaction energies were evaluated using HF/3–21 G energy frameworks analysis. Structural parameters were compared to those of the chloro-containing analogue, and the effect of substituent variation was discussed.
{"title":"Synthesis, crystal structure, Hirshfeld surface analysis, and energy framework of bis{3-(4-bromophenyl)-5-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-4H-1,2,4-triazol-4-ido}nickel(II) methanol disolvate and comparison with its chloro-substituted analogue","authors":"Kateryna Znovjyak , Sergiu Shova , Sergiy O. Nikitin , Yurii S. Moroz , Oksana Tananaiko , Sergey O. Malinkin , Maksym Seredyuk","doi":"10.1107/S2056989025007467","DOIUrl":"10.1107/S2056989025007467","url":null,"abstract":"<div><div>The title compound, a neutral bis{3-(4-bromophenyl)-5-[6-(1<em>H</em>-pyrazol-1-yl)pyridin-2-yl]-4<em>H</em>-1,2,4-triazol-4-ido}nickel(II) methanol disolvate, exhibits a distorted pseudooctahedral coordination environment around the metal ion. Due to the conical geometry and polar characteristics the molecules stack in one-dimensional columns that are connected by weak hydrogen bonds to form layers. These layers are arranged in a three-dimensional lattice without interlayer interactions closer than van der Waals distances.</div></div><div><div>The unit cell of the title compound, [Ni(C<sub>16</sub>H<sub>10</sub>BrN<sub>6</sub>)<sub>2</sub>]·2CH<sub>3</sub>OH, contains a neutral complex and two methanol molecules. The Ni<sup>II</sup> ion adopts a pseudooctahedral geometry, coordinated by two tridentate ligands <em>via</em> pyrazole, pyridine, and triazole N atoms. The average Ni—N bond length is 2.097 (4) Å. In the crystal, molecules form supramolecular chains through weak C–H⋯π interactions and further assemble into diperiodic layers <em>via</em> C—H⋯N/C interactions. Hirshfeld surface analysis shows H⋯H (32.1%), H⋯C/C⋯H (27.3%), H⋯N/N⋯H (14.9%), and H⋯Br/Br⋯H (14.6%) contacts. Interaction energies were evaluated using HF/3–21 G energy frameworks analysis. Structural parameters were compared to those of the chloro-containing analogue, and the effect of substituent variation was discussed.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 10","pages":"Pages 906-911"},"PeriodicalIF":0.6,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243524","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 : 2025-10-01DOI: 10.1107/S2056989025005109
Shao-Liang Zheng , Sean Parkin
The Acta Crystallographica Section E announces a call for papers for its new Education and outreach section, dedicated to showcasing innovative practices, resources, and insights in crystallography and structural chemistry education and public engagement.
This editorial announces the launch of the Education and outreach section in Acta Crystallographica Section E, inspired by the success of the 2023 virtual issue on Modern approaches and tools for teaching crystallography. The section invites detailed advice on challenges encountered during structure solution and refinement, as well as tested educational activities, outreach reports, and practical teaching resources in crystallography and structural chemistry, with an emphasis on reproducibility and student involvement. Inaugural contributions are highlighted, and global submissions are welcomed to build a collaborative resource for advancing education in structural science.
{"title":"Empowering learning in crystallography: launch of the Education and outreach section in Acta Crystallographica Section E","authors":"Shao-Liang Zheng , Sean Parkin","doi":"10.1107/S2056989025005109","DOIUrl":"10.1107/S2056989025005109","url":null,"abstract":"<div><div>The <em>Acta Crystallographica Section E</em> announces a call for papers for its new <em>Education and outreach</em> section, dedicated to showcasing innovative practices, resources, and insights in crystallography and structural chemistry education and public engagement.</div></div><div><div>This editorial announces the launch of the <em>Education and outreach</em> section in <em>Acta Crystallographica Section E</em>, inspired by the success of the 2023 virtual issue on <em>Modern approaches and tools for teaching crystallography</em>. The section invites detailed advice on challenges encountered during structure solution and refinement, as well as tested educational activities, outreach reports, and practical teaching resources in crystallography and structural chemistry, with an emphasis on reproducibility and student involvement. Inaugural contributions are highlighted, and global submissions are welcomed to build a collaborative resource for advancing education in structural science.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 10","pages":"Pages 879-881"},"PeriodicalIF":0.6,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243433","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 : 2025-10-01DOI: 10.1107/S2056989025007327
Sean Parkin
A remedy for unusual weighting schemes sometimes encountered in structure refinements with SHELXL is presented, along with a worked example.
In routine small-molecule structure refinements with SHELXL, the default weighting scheme relies on two adjustable parameters, a and b, in the WGHT command. For most refinements the a value is typically <0.1 while b is expected to be <1 or so. High values of a can be a consequence of poor counting statistics, i.e., weak data. Large values of b may result from uncorrected systematic errors and/or unresolved problems, such as missed symmetry, disorder, and twinning. Nevertheless, on occasion large b values persist, even when there are no apparent model deficiencies. In such cases, the available evidence suggests that the uncertainties derived during data reduction are too small. This short tutorial-style paper presents a straightforward means of achieving WGHT parameters within the expected ranges by fine-tuning parameters used in the Bruker data scaling, merging, and absorption correction program SADABS. Thus, it could also provide a basis for further exploration of weighting schemes in SHELXL. The general principles ought to be adaptable to data reduction software from other diffractometer manufacturers.
{"title":"A remedy for unusual SHELXL weighting schemes","authors":"Sean Parkin","doi":"10.1107/S2056989025007327","DOIUrl":"10.1107/S2056989025007327","url":null,"abstract":"<div><div>A remedy for unusual weighting schemes sometimes encountered in structure refinements with <em>SHELXL</em> is presented, along with a worked example.</div></div><div><div>In routine small-molecule structure refinements with <em>SHELXL</em>, the default weighting scheme relies on two adjustable parameters, <em>a</em> and <em>b</em>, in the WGHT command. For most refinements the <em>a</em> value is typically <0.1 while <em>b</em> is expected to be <1 or so. High values of <em>a</em> can be a consequence of poor counting statistics, <em>i.e.</em>, weak data. Large values of <em>b</em> may result from uncorrected systematic errors and/or unresolved problems, such as missed symmetry, disorder, and twinning. Nevertheless, on occasion large <em>b</em> values persist, even when there are no apparent model deficiencies. In such cases, the available evidence suggests that the uncertainties derived during data reduction are too small. This short tutorial-style paper presents a straightforward means of achieving WGHT parameters within the expected ranges by fine-tuning parameters used in the Bruker data scaling, merging, and absorption correction program <em>SADABS</em>. Thus, it could also provide a basis for further exploration of weighting schemes in <em>SHELXL.</em> The general principles ought to be adaptable to data reduction software from other diffractometer manufacturers.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 10","pages":"Pages 882-888"},"PeriodicalIF":0.6,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243475","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 : 2025-10-01DOI: 10.1107/S2056989025008023
Ben. J. Tickner , Richard J. Gammons , Carlos Platas-Iglesias , Adrian C. Whitwood , Simon B. Duckett
The single-crystal X-ray structure analysis of a pentanuclear iridium hydride cluster containing four N-heterocyclic carbenes and a CO ligand was supported by DFT-calculations. The pentanuclear iridium core exhibits a trigonal–bipyramidal structure and the 15 hydride sites show terminal, μ2- and μ3-bridging coordination modes.
The crystal structure of a unique pentanuclear Ir cluster, tetrakis[1,3-bis(2,4,6-trimethylphenyl)-1,3-dihydro-2H-imidazol-2-ylidene-κC2]carbonyldi-μ3-hydrido-tetra-μ2-hydrido-nonahydridopentairidium(III), [Ir5(μ3-H)2(μ2-H)4H9(C21H24N2)4(CO)], has been refined from X-ray data and supported by density functional theory (DFT) calculations. The five iridium(III) sites of the cluster form a trigonal–bipyramidal structure: three are located in the equatorial triangular plane and are capped by axial metal sites above and below the centre of this plane. Four of these iridium atoms are associated with an N-heterocyclic carbene ligand, and a fifth, which is located in the equatorial plane, is bonded to a CO ligand, which must come from the methanol solvent. The 15 hydride ligands in the cluster could not be located in electron-density difference maps and their locations were optimized by using DFT approaches to calculate the lowest energy structure. These methods revealed the presence of nine terminal, four μ2-, and two μ3-bridging hydrides, which unusually cap faces of three metal atoms. The cluster formed from reaction of an IrI precursor with H2 and NaOMe base in methanol, and it likely reflects an example of a catalytic deactivation product when active IrIII hydrogenation, isotope exchange, or signal amplification by reversible exchange (SABRE) catalysts aggregate in solution to form crystalline or other solid-state products.
基于x射线数据，用密度泛函理论（DFT）计算得到了一种独特的五核Ir簇，即四基-[1,3-二-（2,4,6-三甲基-苯基）-1,3-二氢-2-咪唑-2-基-κ c 2]羰基-μ3-羟基-四-μ2-羟基-nona-羟基-铱（III）， [Ir5(μ3-H)2(μ2-H)4H9(C21H24N2)4(CO)]。星团的五个铱（III）位形成一个三角-双锥体结构：三个位于赤道三角形平面上，由平面中心上下的轴向金属位覆盖。其中四个铱原子与一个n杂环羰基配体相连，第五个原子位于赤道面上，与一个CO配体相连，而CO配体必须来自甲醇溶剂。簇中的15个氢化物配体无法在电子密度差图中定位，利用DFT方法计算最低能量结构，优化了它们的位置。这些方法发现了9个末端、4个μ2-和2个μ3-桥接氢化物的存在，它们不同寻常地覆盖在三个金属原子的表面。由IrI前驱体与H2和NaOMe碱在甲醇中反应形成的团簇，它可能反映了催化失活产物的一个例子，当活性IrIII加氢、同位素交换或可逆交换（SABRE）催化剂的信号放大在溶液中聚集形成晶体或其他固态产物。
{"title":"A pentanuclear iridium(III) hydride cluster: aggregation of an iridium(I) precatalyst","authors":"Ben. J. Tickner , Richard J. Gammons , Carlos Platas-Iglesias , Adrian C. Whitwood , Simon B. Duckett","doi":"10.1107/S2056989025008023","DOIUrl":"10.1107/S2056989025008023","url":null,"abstract":"<div><div>The single-crystal X-ray structure analysis of a pentanuclear iridium hydride cluster containing four N-heterocyclic carbenes and a CO ligand was supported by DFT-calculations. The pentanuclear iridium core exhibits a trigonal–bipyramidal structure and the 15 hydride sites show terminal, μ<sub>2</sub>- and μ<sub>3</sub>-bridging coordination modes.</div></div><div><div>The crystal structure of a unique pentanuclear Ir cluster, tetrakis[1,3-bis(2,4,6-trimethylphenyl)-1,3-dihydro-2<em>H</em>-imidazol-2-ylidene-κ<em>C</em><sup>2</sup>]carbonyldi-μ<sub>3</sub>-hydrido-tetra-μ<sub>2</sub>-hydrido-nonahydridopentairidium(III), [Ir<sub>5</sub>(μ<sub>3</sub>-H)<sub>2</sub>(μ<sub>2</sub>-H)<sub>4</sub>H<sub>9</sub>(C<sub>21</sub>H<sub>24</sub>N<sub>2</sub>)<sub>4</sub>(CO)], has been refined from X-ray data and supported by density functional theory (DFT) calculations. The five iridium(III) sites of the cluster form a trigonal–bipyramidal structure: three are located in the equatorial triangular plane and are capped by axial metal sites above and below the centre of this plane. Four of these iridium atoms are associated with an N-heterocyclic carbene ligand, and a fifth, which is located in the equatorial plane, is bonded to a CO ligand, which must come from the methanol solvent. The 15 hydride ligands in the cluster could not be located in electron-density difference maps and their locations were optimized by using DFT approaches to calculate the lowest energy structure. These methods revealed the presence of nine terminal, four μ<sub>2</sub>-, and two μ<sub>3</sub>-bridging hydrides, which unusually cap faces of three metal atoms. The cluster formed from reaction of an Ir<sup>I</sup> precursor with H<sub>2</sub> and NaOMe base in methanol, and it likely reflects an example of a catalytic deactivation product when active Ir<sup>III</sup> hydrogenation, isotope exchange, or signal amplification by reversible exchange (SABRE) catalysts aggregate in solution to form crystalline or other solid-state products.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 10","pages":"Pages 958-963"},"PeriodicalIF":0.6,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145243514","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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