Acta Crystallographica Section E: Crystallographic Communications最新文献

{"title":"Crystal structure of a solvated dinuclear CuII complex derived from 3,3,3′,3′-tetraethyl-1,1′-(furan-2,5-dicarbonyl)bis(thiourea)","authors":"Canh Dinh Le ,&nbsp;Hoang Phuc Nguyen ,&nbsp;Chien Thang Pham","doi":"10.1107/S2056989024010703","DOIUrl":"10.1107/S2056989024010703","url":null,"abstract":"<div><div>In the title compound, [Cu₂(<em>L</em>)₂]·2CH₂Cl₂, the Cu^II ions coordinate two (<em>S</em>,<em>O</em>)-chelating aroyl­thio­urea moieties of doubly deprotonated furan-2,5-di­carbonyl­bis­(<em>N</em>,<em>N</em>-di­ethyl­thio­urea) (<strong>H₂L</strong>) ligands. The coordination geometry of the metal centers is best described as a flat isosceles trapezoid with a <em>cis</em> arrangement of the donor atoms.</div></div><div><div>Reaction between equimolar amounts of 3,3,3′,3′-tetraethyl-1,1′-(furan-2,5-dicarbonyl)bis(thiourea) (<strong>H₂L</strong>) and CuCl₂·2H₂O in methanol in the presence of the supporting base Et₃N gave rise to a neutral dinuclear complex bis­[μ-3,3,3′,3′-tetraethyl-1,1′-(furan-2,5-dicarbonyl)bis(thioureato)]dicopper(II) di­chloro­methane disolvate, [Cu₂(C₁₆H₂₂N₄O₃S₂)₂]·2CH₂Cl₂ or [Cu₂(<em>L</em>)₂]·2CH₂Cl₂. The aroylbis(thio­ureas) are doubly deprotonated and the resulting anions {<em>L</em>^2–} bond to metal ions through (<em>S</em>,<em>O</em>)-chelating moieties. The copper atoms adopt a virtually <em>cis</em>-square-planar environment. In the crystal, adjacent [Cu₂(<em>L</em>)₂]·2CH₂Cl₂ units are linked into polymeric chains along the <em>a-</em>axis direction by inter­molecular coordinative Cu⋯S inter­actions. The co-crystallized solvent mol­ecules play a vital role in the crystal packing. In particular, weak C—H_furan⋯Cl and C—H_eth­yl⋯Cl contacts consolidate the three-dimensional supra­mol­ecular architecture.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1266-1269"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129709","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comprehensive structural study of lanthanide(III) chloride hydrates: [RECl3·xH2O (RE = La–Nd, Sm–Lu; x = 6, 7)]","authors":"Thimira Kandabadage ,&nbsp;Beau Legnon ,&nbsp;Sviatoslav Baranets","doi":"10.1107/S2056989024011319","DOIUrl":"10.1107/S2056989024011319","url":null,"abstract":"<div><div>This study presents a comprehensive crystallographic analysis of the lanthanide(III) chloride hydrates [<em>RE</em>Cl₃·xH₂O (<em>RE</em> = La–Nd, Sm–Lu; <em>x</em> = 6, 7)], offering new structural data for the series. The research highlights the influence of hydration levels and lanthanide contraction on the crystal structures, while identifying missing data for specific hydrates in existing structural databases.</div></div><div><div>A comprehensive crystallographic study is presented of the complete series of rare-earth(III) chloride hydrates. Early lanthanides form dimeric [(H₂O)₇<em>RE</em>(μ-Cl)₂<em>RE</em>(H₂O)₇]⁴⁺ binuclear complexes in which each <em>RE</em> atom (<em>RE</em> = La³⁺, Ce³⁺) is coordinated by seven H₂O mol­ecules and two bridging inner-sphere chloride ions. Di-μ-chlorido-bis­[hepta­aqua­lanthanide(III)] tetra­chloride, [(H₂O)₇<em>RE</em>(μ-Cl)₂<em>RE</em>(H₂O)₇]Cl₄, crystallizes in the triclinic space group <em>P</em>1. Heavier lanthanides exhibit monomeric [<em>RE</em>Cl₂(H₂O)₆]⁺ units where each <em>RE</em> atom (<em>RE</em> = Pr³⁺, Nd³⁺, Sm³⁺–Lu³⁺) is coordinated by six H₂O mol­ecules and two inner-sphere chloride ions. Hexa­aqua­dichlorido­lanthanide(III) chlorides, [<em>RE</em>Cl₂(H₂O)₆]Cl, adopt the monoclinic space group <em>P</em>2/<em>c.</em> In both structures, the cationic <em>inner-sphere</em> complex is counter-charged by the corresponding number of <em>outer-sphere</em> Cl⁻ anions, in which the metal ion and outer-sphere chloride ion lie on crystallographic twofold axes. Crystal structures for all compounds were determined in high quality with refined H-atom positions and were collected at the same temperature (100 K), providing a uniform structural dataset and addressing discrepancies in previous reports. The crystal structure of [HoCl₂(H₂O)₆]Cl is reported for the first time.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1342-1349"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129257","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal structure and Hirshfeld-surface analysis of an etoxazole metabolite designated R13","authors":"Thaluru M. Mohan Kumar ,&nbsp;Besagarahally L. Bhaskar ,&nbsp;Prabhakar Priyanka ,&nbsp;Thayamma R. Divakara ,&nbsp;Hemmige S. Yathirajan ,&nbsp;Sean Parkin","doi":"10.1107/S2056989024010600","DOIUrl":"10.1107/S2056989024010600","url":null,"abstract":"<div><div>The crystal structure of a metabolite of the insecticide/acaricide etoxazole, designated R13 is presented along with a Hirshfeld surface analysis of inter­molecular inter­actions present in the crystal structure.</div></div><div><div>The etoxazole metabolite <strong>R13</strong>, systematic name 4-(4-<em>tert</em>-butyl-2-eth­oxy­phen­yl)-2-(2,6-di­fluoro­phen­yl)oxazole (C₂₁H₂₁F₂NO₂), results from the oxidation of etoxazole, a chitin synthesis inhibitor belonging to the oxazoline class, widely used as an insecticide/acaricide since 1998. The structure of <strong>R13</strong> features a central oxazole ring with attached 2,6-di­fluoro­phenyl and 4-<em>t</em>-butyl-2-eth­oxy­phenyl moieties. The overall conformation gives dihedral angles between these rings and the oxazole of 24.91 (5)° (with di­fluoro­phen­yl) and 15.30 (6)° (with <em>t</em>-butyl-eth­oxy­phen­yl), indicating an overall deviation from planarity. Additionally, torsion angles of the eth­oxy and <em>t</em>-butyl groups define the orientation of these substituents relative to their benzene ring. In the crystal packing, no significant hydrogen bonds are present, but a Hirshfeld surface analysis highlights weak inter­molecular contacts leading to π–π-stacked dimers linked by weak C—H⋯N contacts. The packing analysis confirms that most inter­molecular inter­actions involve hydrogen atoms.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1270-1273"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129416","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal structure of 1,10-phenanthrolinium violurate violuric acid penta­hydrate","authors":"Rüdiger W. Seidel ,&nbsp;Tsonko M. Kolev","doi":"10.1107/S205698902401065X","DOIUrl":"10.1107/S205698902401065X","url":null,"abstract":"<div><div>The crystal structure of the co-crystal salt solvate 1,10-phenanthrolinium violurate violuric acid penta­hydrate features a tri-periodic hydrogen-bonded network with the violurate and violuric acid residues each assembled into tapes and the phenanthrolinium cations residing in channels.</div></div><div><div>The title compound [systematic name: 1,10-phenanthrolinium 6-hy­droxy-5-(oxido­imino)-1,3-diazinane-2,4-dione–6-hy­droxy-5-(hy­droxy­imino)-1,3-diazin­ane-2,4-dione–water (1/1/5)], C₁₂H₉N₂⁺·C₄H₂N₃O₄⁻·C₄H₃N₃O₄·5H₂O, is a co-crystal salt hydrate comprising 1,10-phenanthrolinium cations, violurate anions, free violuric acid as co-former and five water mol­ecules of crystallization per formula unit. The violurate and the violuric acid residues each form distinct N—H⋯O hydrogen-bonded tapes with a common <em>R</em>²₂(8) hydrogen-bond motif extending parallel to (103). Solvent water mol­ecules connect the tapes to form a tri-periodic hydrogen-bonded network with channels extending parallel to the <em>a</em>-axis direction, which accommodate the N—H⋯O_water hydrogen-bonded 1,10-phenanthrolinium cations. Direct N—H⋯O hydrogen bonds between the 1,10-phenanthrolinium and violurate ions are not encountered.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1288-1292"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129249","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Syntheses and crystal structures of (R,R)- and (S,S)-bis­(aceto­nitrile-κN)[N,N′-dimethyl-N,N′-bis(pyridin-2-ylmeth­yl)cyclo­hexane-1,2-di­amine-κ4N]iron(II) bis­(hexa­fluoro­anti­monate)","authors":"Yurii S. Bibik ,&nbsp;Iryna M. Yulakh ,&nbsp;Svitlana V. Shishkina ,&nbsp;Dmytro M. Khomenko ,&nbsp;Roman O. Doroshchuk ,&nbsp;Ilona V. Raspertova ,&nbsp;Rostyslav D. Lampeka","doi":"10.1107/S2056989024011307","DOIUrl":"10.1107/S2056989024011307","url":null,"abstract":"<div><div>The syntheses and crystal structures of two enanti­omeric non-heme iron catalysts based on <em>N</em>,<em>N</em>′-dimethyl-<em>N</em>,<em>N</em>′-bis­(pyridin-2-ylmeth­yl)cyclo­hexane-1,2-di­amine are described.</div></div><div><div>Two enanti­omeric non-heme iron complexes [Fe(<em>R</em>,<em>R</em>-BPMCN)(CH₃CN)₂](SbF₆)₂ and [Fe(<em>S</em>,<em>S</em>-BPMCN)(CH₃CN)₂](SbF₆)₂ (BPMCM = <em>N</em>,<em>N</em>′-dimethyl-<em>N</em>,<em>N</em>′-bis­(pyridin-2-ylmeth­yl)-cyclo­hexane-1,2-di­amine, C₂₂H₂₈N₄) were obtained in parallel syntheses starting from the enanti­omerically pure <em>R</em>,<em>R</em> and <em>S</em>,<em>S</em> BPMCN ligands. The Fe^II cations have a distorted octa­hedral FeN₆ geometry formed by a chelating <em>N</em>,<em>N</em>,<em>N</em>,<em>N</em>-tetra­dentate BPMCN ligand and two mol­ecules of aceto­nitrile. The ligand adopts a <em>cis</em>-<em>α</em> topology with the two pyridine groups coordinated <em>trans</em> to each other. In the crystals, a system of C—H⋯F hydrogen bonds links the cations to the hexa­fluoro­anti­monate anions, resulting in a three-dimensional architecture.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1350-1353"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129417","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal structures of two polymorphs for fac-bromido­tricarbon­yl[4-(4-meth­oxy­phen­yl)-2-(pyridin-2-yl)thia­zole-κ2N,N′]rhenium(I)","authors":"Yuki Matsuda ,&nbsp;Ryota Nakamura ,&nbsp;Yoshiki Ozawa ,&nbsp;Masaaki Abe","doi":"10.1107/S2056989024010727","DOIUrl":"10.1107/S2056989024010727","url":null,"abstract":"<div><div>Crystallization of the title compound from CH₂Cl₂/<em>n</em>-pentane (1:5 <em>v</em>/<em>v</em>) at room temperature gave two polymorphs, which crystallize in monoclinic (<em>P</em>2₁/<em>c</em>; α form) and ortho­rhom­bic (<em>Pna</em>2₁; β form) space groups. The Re^I complex mol­ecules in either polymorph adopt a six-coordinate octa­hedral geometry with three <em>facially</em>-oriented carbonyl ligands, one bromido ligand, and two nitro­gen atoms from one chelating ligand ppt-OMe. In the crystal, both polymorph α and β form di-periodic sheet-like architectures supported by multiple hydrogen bonds.</div></div><div><div>Crystallization of the title compound, <em>fac</em>-[ReBr(ppt-OMe)(CO)₃] (ppt-OMe = C₁₅H₁₂N₂OS), from CH₂Cl₂/<em>n</em>-pentane (1:5 <em>v</em>/<em>v</em>) at room temperature gave two polymorphs, which crystallize in monoclinic (<em>P</em>2₁/<em>c</em>; α form) and ortho­rhom­bic (<em>Pna</em>2₁; β form) space groups. The Re^I complex mol­ecules in either polymorph adopt a six-coordinate octa­hedral geometry with three <em>facially</em>-oriented carbonyl ligands, one bromido ligand, and two nitro­gen atoms from one chelating ligand ppt-OMe. In the crystal, both polymorph α and β form di-periodic sheet-like architectures supported by multiple hydrogen bonds. In polymorph α, two types of hydrogen bonds (C—H⋯O) are found while, in polymorph β, four types of hydrogen bonds (C—H⋯O and C—H⋯Br) exist.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1283-1287"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129745","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal structures and circular dichroism of {2,2′-[(1S,2S)-1,2-di­phenyl­ethane-1,2-diylbis(nitrilophenyl­methanylyl­idene)]diphenolato}nickel(II) and its ethanol solvate","authors":"Masataka Ito ,&nbsp;Noriko Chikaraishi Kasuga ,&nbsp;Ryo Matsuse ,&nbsp;Masakazu Hirotsu","doi":"10.1107/S2056989024010508","DOIUrl":"10.1107/S2056989024010508","url":null,"abstract":"<div><div>A chiral nickel(II) Schiff base complex derived from 2-hy­droxy­benzo­phenone and (1<em>S</em>,2<em>S</em>)-1,2-di­phenyl­ethyl­enedi­amine shows a λ conformation of the central di­amine chelate ring. The substituents on the C=N carbon atoms significantly affect the circular dichroism spectra.</div></div><div><div>The title compound, [Ni(C₄₀H₃₀N₂O₂)] (<strong>1</strong>), with an optically active Schiff base ligand derived from 2-hy­droxy­benzo­phenone and (1<em>S</em>,2<em>S</em>)-1,2-di­phenyl­ethyl­enedi­amine, was crystallized as the solvent-free and ethanol solvate forms (<strong>1</strong> and <strong>1</strong>·2C₂H₅OH). In both structures, the two phenyl groups on the stereogenic centers of the <em>O</em>,<em>N</em>,<em>N</em>,<em>O</em>-tetra­dentate ligand are axially oriented, and the conformation of the central di­amine chelate ring is λ. The circular dichroism (CD) spectra of <strong>1</strong> and the analogous nickel(II) complex [Ni(C₃₀H₂₆N₂O₂)] (<strong>2</strong>) in solution show partially similar patterns in the 350–450 nm range, but are mirror images in the longer wavelength region (450–650 nm). In the latter region, the sign of CD for these complexes is sensitive to the substituents on the C=N carbon atoms (phenyl for <strong>1</strong> and methyl for <strong>2</strong>) rather than the di­amine chelate ring conformation.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1259-1265"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129890","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Syntheses and crystal structures of the imides 4-(2-phenyl­eth­yl)- and 4-[2-(4-hy­droxy­phen­yl)eth­yl]-4-aza­tetra­cyclo­[5.3.2.02,6.08,10]dodec-11-ene-3,5-dione","authors":"Jonathan P. Bajko ,&nbsp;Richard J. Staples ,&nbsp;Shannon M. Biros","doi":"10.1107/S2056989024011253","DOIUrl":"10.1107/S2056989024011253","url":null,"abstract":"<div><div>The crystal structures of the title compounds feature C—H⋯π inter­actions as well as O—H⋯O and C—H⋯O hydrogen bonds.</div></div><div><div>The syntheses and characterization (NMR and XRD) of two substituted [2.2.2]bi­cyclo­octene ring systems are described here. The cyclo­hexene rings of these systems adopt a nearly perfect boat conformation according to analysis using Cremer–Pople parameters. Both structures contain a nearly planar imide ring that is oriented <em>endo</em> relative to a bridgehead cyclo­propyl ring. 4-(2-Phenyl­eth­yl)-4-aza­tetra­cyclo­[5.3.2.0^2,6.0^8,10]dodec-11-ene-3,5-dione, C₁₉H₁₉NO₂, is substituted with a phenylethyl group that hosts C—H⋯π inter­actions in the crystal. 4-[2-(4-Hy­droxy­phen­yl)eth­yl]-4-aza­tetra­cyclo­[5.3.2.0^2,6.0^8,10]dodec-11-ene-3,5-dione, C₁₉H₁₉NO₃, bears a 4-hy­droxy­phenylethyl group on the imide ring and contains O—H⋯O and C—H⋯O hydrogen bonds.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1318-1321"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143130064","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal structure of the 1:1 cocrystal 5,5′-(triaz-1-ene-1,3-di­yl)bis­(3-nitro-1H-1,2,4-triazole)–tri­ethylammonium nitrate","authors":"Matthew Gettings ,&nbsp;Matthias Zeller ,&nbsp;Davin Piercey","doi":"10.1107/S205698902401096X","DOIUrl":"10.1107/S205698902401096X","url":null,"abstract":"<div><div>The tri­ethyl­ammonium nitrate cocrystal of 5,5′-(triaz-1-ene-1,3-di­yl)bis­(3-nitro-1<em>H</em>-1,2,4-triazole), obtained unintentionally from 3-amino-5-nitro-1,2,4-triazole (ANTA), exhibits extensive hydrogen bonding and modulation by pseudo-translation with <em>Z</em>* = 4.</div></div><div><div>The tri­ethyl­ammonium nitrate cocrystal of 5,5′-(triaz-1-ene-1,3-di­yl)bis­(3-nitro-1<em>H</em>-1,2,4-triazole), C₄H₃N₁₁O₄·C₆H₁₆N·NO₃ (<strong>3</strong>), was obtained unintentionally as the product of an attempted synthesis of a heterocyclic <em>C</em>-bromo­nitrilimine from 3-amino-5-nitro-1,2,4-triazole (ANTA). In the solid state at 150 K, the structure of <strong>3</strong> is modulated by a pseudo-translation along [010] with <em>Z</em>* = 4 (<em>Z</em> = 8 in <em>P</em>1). Exact translational symmetry is broken by a slight modulation of the triazene mol­ecules and nitrate anions, and by disorder of two of the four tri­ethyl­ammonium cations. An extensive hydrogen-bonding network connects the components of the structure and enables a relatively high density of 1.516 g cm⁻³. This feature, as well as its high nitro­gen content, make this rare triazene-bridged 1,2,4-triazole and possible related similar compounds of inter­est as potential energetic materials.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1302-1307"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129746","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal structure, Hirshfeld surface analysis, DFT and mol­ecular docking studies of ethyl 5-amino-2-bromo­isonicotinate","authors":"Harish Kumar Mahadevaiah ,&nbsp;Harishkumar Shivanna ,&nbsp;Anil Kumar Hanumaiah ,&nbsp;Devarajegowda Hirehalli Chikkegowda ,&nbsp;Palakshamurthy Bandrehalli Siddagangaiah","doi":"10.1107/S2056989024010594","DOIUrl":"10.1107/S2056989024010594","url":null,"abstract":"<div><div>Theoretical and experimental structural studies of the title compound were undertaken using X-ray and DFT methods. The inter­actions present in the crystal were analyzed using Hirshfeld surface and MEP surface analysis. Docking studies with a covid-19 main protease (PDB ID: 6LU7) as the target receptor indicate that the synthesized compound may be a potential candidate for pharmaceutical applications.</div></div><div><div>In the title compound, C₈H₉BrN₂O₂, the C—O—C—C torsion angle between isonicotine and the ethyl group is 180.0 (2)°. Intra­molecular N—H⋯O and C—H⋯O inter­actions consolidate the mol­ecular structure. In the crystal, N—H⋯N inter­action form <em>S</em>(5) zigzag chains along [010]. The most significant contributions to the Hirshfeld surface arise from H⋯H (33.2%), Br⋯H/H⋯Br (20.9%), O⋯H/H⋯O (11.2%), C⋯H/H⋯C (11.1%) and N⋯H/H⋯N (10%) contacts. The topology of the three-dimensional energy frameworks was generated using the B3LYP/6–31 G(d,p) model to calculate the total inter­action energy. The net inter­action energies for the title compound are <em>E</em>_ele = 59.2 kJ mol⁻¹, <em>E</em>_pol = 15.5 kJ mol⁻¹, <em>E</em>_dis = 140.3 kJ mol⁻¹ and <em>E</em>_rep = 107.2 kJ mol⁻¹ with a total inter­action energy <em>E</em>_tot of 128.8 kJ mol⁻¹. The mol­ecular structure was optimized by density functional theory (DFT) at the B3LYP/6–311+G(d,p) level and the theoretical and experimentally obtained parameters were compared. The frontier mol­ecular orbitals HOMO and LUMO were generated, giving an energy gap Δ<em>E</em> of 4.0931 eV. The MEP was generated to identify active sites in the mol­ecule and mol­ecular docking studies carried out with the title compound (ligand) and the covid-19 main protease PDB ID: 6LU7, revealing a moderate binding affinity of −5.4 kcal mol⁻¹.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 12","pages":"Pages 1274-1279"},"PeriodicalIF":0.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143129253","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}