Acta Crystallographica Section E: Crystallographic Communications最新文献

{"title":"Crystal structure and Hirshfeld-surface analysis of the pesticide etoxazole","authors":"Chaluvarangaiah Sowbhagya ,&nbsp;Thaluru M. Mohan Kumar ,&nbsp;Hemmige S. Yathirajan ,&nbsp;Sean Parkin","doi":"10.1107/S2056989025001173","DOIUrl":"10.1107/S2056989025001173","url":null,"abstract":"<div><div>The crystal structure of the insecticide/acaricide etoxazole is presented along with a Hirshfeld surface analysis of inter­molecular inter­actions present in the crystal structure.</div></div><div><div>Etoxazole (C₂₁H₂₃F₂NO₂), systematic name 4-(4-<em>tert</em>-butyl-2-eth­oxy­phen­yl)-2-(2,6-di­fluoro­phen­yl)-4,5-di­hydro-1,3-oxazole, is a fluorinated insecticide and acaricide that inhibits chitin biosynthesis, disrupting insect development by preventing proper exoskeleton formation. Widely used in agriculture since 1998, it is readily absorbed by plant tissues and translocates within leaves. Metabolic studies have identified several oxidative degradation products, while toxicol­ogical assessments have examined potential effects, including oxidative stress. This study presents a detailed crystallographic and Hirshfeld surface analysis of etoxazole. The mol­ecule consists of a central di­hydro-oxazole ring flanked by 2,6-di­fluoro­phenyl and 4-<em>tert</em>-butyl-2-eth­oxy­phenyl groups, each twisted relative to the oxazole core. The di­hydro-oxazole ring is nearly planar, with the substituted phenyl rings forming dihedral angles of 44.20 (4)° and 47.87 (4)° with the mean plane of the di­hydro-oxazole. The eth­oxy group exhibits a dihedral angle of 15.04 (11)° to the <em>tert</em>-butyl­phenyl ring, while the <em>tert</em>-butyl group itself shows minor torsional disorder [major:minor occupancies are 0.760 (6):0.240 (6)]. The mol­ecular packing is dominated by van der Waals-type inter­actions, though weak C—H⋯F and C—H⋯O inter­actions lead to pleated layers parallel to the <em>ab</em> plane, which further stack along the <em>c</em>-axis direction. A Hirshfeld surface analysis confirms the prevalence of van der Waals inter­actions in crystal stabilization.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 239-242"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891584/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603376","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 six complexes of phosphane chalcogenides R1R2R3PE (R = tert-butyl or isopropyl, E = S or Se) with the metal halides MX2 (M = Pd or Pt, X = Cl or Br), two halochalcogenyl­phospho­nium derivatives (tBu2iPrPEBr)2[Pd2Br6] and one hydrolysis product","authors":"Daniel Upmann ,&nbsp;Peter G. Jones","doi":"10.1107/S2056989025000805","DOIUrl":"10.1107/S2056989025000805","url":null,"abstract":"&lt;div&gt;&lt;div&gt;Various compounds involving tri­alkyl­phosphane chalcogenides (or their derivatives) and palladium or platinum dihalides were structurally characterized and their intra- and inter­molecular inter­actions and metrical parameters were analysed. General comments on the SFAC command are also included.&lt;/div&gt;&lt;/div&gt;&lt;div&gt;&lt;div&gt;The &lt;em&gt;L&lt;/em&gt;&lt;sub&gt;2&lt;/sub&gt;&lt;em&gt;MX&lt;/em&gt;&lt;sub&gt;2&lt;/sub&gt; complexes &lt;strong&gt;1&lt;/strong&gt;–&lt;strong&gt;5&lt;/strong&gt; (&lt;strong&gt;1&lt;/strong&gt;: &lt;em&gt;L&lt;/em&gt; = &lt;sup&gt;&lt;em&gt;t&lt;/em&gt;&lt;/sup&gt;Bu&lt;sup&gt;i&lt;/sup&gt;Pr&lt;sub&gt;2&lt;/sub&gt;PSe, &lt;em&gt;M&lt;/em&gt; = Pd, &lt;em&gt;X&lt;/em&gt; = Cl; &lt;strong&gt;2&lt;/strong&gt;: &lt;em&gt;L&lt;/em&gt; = &lt;sup&gt;&lt;em&gt;t&lt;/em&gt;&lt;/sup&gt;Bu&lt;sub&gt;2&lt;/sub&gt;&lt;sup&gt;i&lt;/sup&gt;PrPSe, &lt;em&gt;M&lt;/em&gt; = Pd, &lt;em&gt;X&lt;/em&gt; = Cl; &lt;strong&gt;3&lt;/strong&gt;: &lt;em&gt;L&lt;/em&gt; = &lt;sup&gt;&lt;em&gt;t&lt;/em&gt;&lt;/sup&gt;Bu&lt;sub&gt;2&lt;/sub&gt;&lt;sup&gt;i&lt;/sup&gt;PrPSe, &lt;em&gt;M&lt;/em&gt; = Pd, &lt;em&gt;X&lt;/em&gt; = Br; &lt;strong&gt;4&lt;/strong&gt;: &lt;em&gt;L&lt;/em&gt; = &lt;sup&gt;&lt;em&gt;t&lt;/em&gt;&lt;/sup&gt;Bu&lt;sub&gt;2&lt;/sub&gt;&lt;sup&gt;i&lt;/sup&gt;PrPS, &lt;em&gt;M&lt;/em&gt; = Pd, &lt;em&gt;X&lt;/em&gt; = Br; &lt;strong&gt;5&lt;/strong&gt;: &lt;em&gt;L&lt;/em&gt; = &lt;sup&gt;&lt;em&gt;t&lt;/em&gt;&lt;/sup&gt;Bu&lt;sub&gt;2&lt;/sub&gt;&lt;sup&gt;i&lt;/sup&gt;PrPS, &lt;em&gt;M&lt;/em&gt; = Pt, &lt;em&gt;X&lt;/em&gt; = Cl) {systematic names: (&lt;em&gt;tert&lt;/em&gt;-butyl­diiso­propyl­phosphine selenide-κ&lt;em&gt;Se&lt;/em&gt;)di­chlorido­palladium(II), [PdCl&lt;sub&gt;2&lt;/sub&gt;(C&lt;sub&gt;10&lt;/sub&gt;H&lt;sub&gt;23&lt;/sub&gt;PSe)&lt;sub&gt;2&lt;/sub&gt;] (&lt;strong&gt;1&lt;/strong&gt;), (di-&lt;em&gt;tert&lt;/em&gt;-butyl­iso­propyl­phosphine selenide-κ&lt;em&gt;Se&lt;/em&gt;)di­chloridopalladium(II), [PdCl&lt;sub&gt;2&lt;/sub&gt;(C&lt;sub&gt;11&lt;/sub&gt;H&lt;sub&gt;25&lt;/sub&gt;PSe)&lt;sub&gt;2&lt;/sub&gt;] (&lt;strong&gt;2&lt;/strong&gt;), di­bromido­(di-&lt;em&gt;tert&lt;/em&gt;-butyl­iso­propyl­phosphine selenide-κ&lt;em&gt;Se&lt;/em&gt;)palladium(II), [PdBr&lt;sub&gt;2&lt;/sub&gt;(C&lt;sub&gt;11&lt;/sub&gt;H&lt;sub&gt;25&lt;/sub&gt;PSe)&lt;sub&gt;2&lt;/sub&gt;] (&lt;strong&gt;3&lt;/strong&gt;), di­bromido­(di-&lt;em&gt;tert&lt;/em&gt;-butyl­iso­propyl­phosphine sulfide-κ&lt;em&gt;S&lt;/em&gt;)palladium(II), [PdBr&lt;sub&gt;2&lt;/sub&gt;(C&lt;sub&gt;11&lt;/sub&gt;H&lt;sub&gt;25&lt;/sub&gt;PS)&lt;sub&gt;2&lt;/sub&gt;] (&lt;strong&gt;4&lt;/strong&gt;), di­chlorido­(di-&lt;em&gt;tert&lt;/em&gt;-butyl­iso­propyl­phosphine sulfide-κ&lt;em&gt;S&lt;/em&gt;)palladium(II), [PdCl&lt;sub&gt;2&lt;/sub&gt;(C&lt;sub&gt;11&lt;/sub&gt;H&lt;sub&gt;25&lt;/sub&gt;PS)&lt;sub&gt;2&lt;/sub&gt;] (&lt;strong&gt;5&lt;/strong&gt;)} all display a &lt;em&gt;trans&lt;/em&gt; configuration with square-planar geometry at the metal atom. Compounds &lt;strong&gt;2&lt;/strong&gt; and &lt;strong&gt;3&lt;/strong&gt; are isotypic. The mol­ecules of &lt;strong&gt;1&lt;/strong&gt; and &lt;strong&gt;4&lt;/strong&gt; display crystallographic inversion symmetry; compound &lt;strong&gt;5&lt;/strong&gt; involves two independent mol­ecules, each with inversion symmetry but with differing orientations of the tri­alkyl­phosphane groups. Chemically equivalent bond lengths all lie in narrow ranges, whereby the values for palladium and platinum compounds scarcely differ. Compound &lt;strong&gt;6&lt;/strong&gt;, (&lt;sup&gt;&lt;em&gt;t&lt;/em&gt;&lt;/sup&gt;Bu&lt;sup&gt;i&lt;/sup&gt;Pr&lt;sub&gt;2&lt;/sub&gt;PS)&lt;sub&gt;2&lt;/sub&gt;Pd&lt;sub&gt;2&lt;/sub&gt;Cl&lt;sub&gt;4&lt;/sub&gt; {systematic name: di-μ-chlorido-bis­[(&lt;em&gt;tert&lt;/em&gt;-butyldiiso­propyl­phosphine sulfide-κ&lt;em&gt;S&lt;/em&gt;)chlorido­palladium(II)], [PdCl&lt;sub&gt;2&lt;/sub&gt;(C&lt;sub&gt;10&lt;/sub&gt;H&lt;sub&gt;23&lt;/sub&gt;PS)&lt;sub&gt;2&lt;/sub&gt;]}, is dinuclear with a central Pd&lt;sub&gt;2&lt;/sub&gt;Cl&lt;sub&gt;2&lt;/sub&gt; ring, and displays crystallographic inversion symmetry. The bonds to the bridging are longer than those to the terminal chlorine atom","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 183-194"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891585/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603199","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":"Synthesis, structural characterization, Hirshfeld surface analysis and QTAIM analysis of 3-(4-cyano­thio­phen-3-yl)-[1,2,4]selena­diazolo[4,5-a]pyridin-4-ium chloride","authors":"Alexander A. Sapronov ,&nbsp;Evgeny A. Dukhnovsky ,&nbsp;Alexey S. Kubasov ,&nbsp;Alexander S. Novikov ,&nbsp;Maria M. Grishina ,&nbsp;Ekaterina V. Dobrokhotova ,&nbsp;Milena R. Komarovskikh ,&nbsp;Namiq Q. Shikhaliyev ,&nbsp;Mehmet Akkurt ,&nbsp;Ajaya Bhattarai ,&nbsp;Alexander G. Tskhovrebov","doi":"10.1107/S205698902500115X","DOIUrl":"10.1107/S205698902500115X","url":null,"abstract":"<div><div>The title compound was produced by the reaction between 3,4-di­cyano­thio­phene and 2-pyridyl­selenyl chloride and isolated as a salt that crystallizes in the triclinic space group <em>P</em>1. Notable features include strong chalcogen inter­actions (Se⋯Cl and Se⋯S), as revealed through Hirshfeld surface analysis, which also highlights significant contributions from N⋯H/H⋯N, C⋯H/H⋯C and H⋯H contacts in the crystal packing.</div></div><div><div>The title compound, C₁₁H₆N₃SSe⁺·Cl⁻, produced by the reaction between 3,4-di­cyano­thio­phene and 2-pyridyl­selenyl chloride was isolated as a salt that crystallizes in the triclinic space group <em>P</em>1. Notable features include strong chalcogen inter­actions (Se⋯Cl and Se⋯S), as revealed through Hirshfeld surface analysis, which also highlights significant contributions from N⋯H/H⋯N, C⋯H/H⋯C and H⋯H contacts in the crystal packing. Supra­molecular inter­actions were further analysed using density functional theory (DFT) and quantum theory of atoms in mol­ecules (QTAIM) at the ωB97XD/6–311++G** level of theory.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 224-228"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891582/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603308","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":"Supra­molecular assembly of mebendazolium and di­hydrogen phosphate ions in a new anthelmintic salt","authors":"Eduardo L. Gutiérrez ,&nbsp;Marcos G. Russo ,&nbsp;Griselda E. Narda ,&nbsp;Elena V. Brusau ,&nbsp;Alejandro P. Ayala ,&nbsp;Javier Ellena","doi":"10.1107/S2056989025000714","DOIUrl":"10.1107/S2056989025000714","url":null,"abstract":"<div><div>A new mebendazolium di­hydrogen phosphate phospho­ric acid solid compound was obtained. As expected, the mebendazolium cation and the di­hydrogen phosphate anion assemble in the solid state in an <em>R</em>₂²(8) hydrogen-bond-driven supra­molecular motif.</div></div><div><div>A new mebendazolium di­hydrogen phosphate phospho­ric acid solid material was obtained and characterized by single-crystal X-ray diffraction and complementary solid-state techniques {systematic name: 5-benzoyl-2-[(meth­oxy­carbon­yl)amino]-1<em>H</em>-1,3-benzo­diazol-3-ium di­hydrogen phosphate–phos­pho­ric acid (1/1), C₁₆H₁₄N₃O₃⁺·H₂PO₄⁻·H₃PO₄}. Structure solution confirmed proton transfer from phospho­ric acid towards the basic imidazole ring of mebendazole. The mebendazolium cation and the di­hydrogen phosphate anion assemble in the solid state in a cyclic hydrogen-bond-driven supra­molecular motif, as observed in all mebendazolium/oxyanions structures reported in the literature. This salt crystallizes in the monoclinic <em>P</em>2₁/<em>c</em> (No. 14) space group. A detailed study of the crystal structure performed by atom-to-atom and global Hirshfeld surface analysis indicates that several hydrogen bonds act as the main inter­molecular inter­actions stabillizing the material. The new material is stable up to 458 K.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 195-199"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891589/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603301","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-[(4-chloro­phen­yl)di­phenylyl­meth­yl]-3-(tri­fluoro­meth­yl)-1H-pyrazole","authors":"Firudin I. Guseinov ,&nbsp;Ksenia A. Afanaseva ,&nbsp;Vera A.Vil ,&nbsp;Bogdan I. Ugrak ,&nbsp;Aida I. Samigullina ,&nbsp;Ennio Zangrando ,&nbsp;Alebel N. Belay","doi":"10.1107/S2056989025001185","DOIUrl":"10.1107/S2056989025001185","url":null,"abstract":"<div><div>The title pyrazole derivative, which exhibits multiple inter­molecular non-covalent inter­actions, was synthesized by the reaction of 3-(tri­fluoro­meth­yl)-1<em>H</em>-pyrazole with chloro­(4-chloro­phen­yl)methyl­ene)di­benzene in the presence of K₂CO₃ in tetra­hydro­furan.</div></div><div><div>The title compound, C₂₃H₁₆ClF₃N₂, was synthesized from 3-(tri­fluoro­meth­yl)-1<em>H</em>-pyrazole and chloro­(4-chloro­phen­yl)methyl­ene)di­benzene. The structure features intra­molecular (Ph)C—H⋯N and inter­molecular (Ph)C—H⋯F hydrogen bonds, as well as C—H⋯π-ring inter­actions between the phenyl and pyrazole rings.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 235-238"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891583/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603108","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":"Synthesis and structure of 2-oxo-2H-chromen-4-yl 4-bromo­benzoate: work carried out as part of the CNRS AFRAMED project","authors":"Valentin Bationo ,&nbsp;Konan René Kambo ,&nbsp;Brahima Sorgho ,&nbsp;Charles Bavouma Sombié ,&nbsp;El Walda Thiam ,&nbsp;Rasmané Semdé ,&nbsp;Abdoulaye Djandé ,&nbsp;Claude Lecomte ,&nbsp;Emmanuel Wenger","doi":"10.1107/S2056989025000246","DOIUrl":"10.1107/S2056989025000246","url":null,"abstract":"<div><div>In the title compound, the dihedral angle between the chromen-2-one ring system and the bromo­benzene ring is 10.29 (6)°. In the crystal, the mol­ecules are connected through C—H⋯O hydrogen bonds and π–π stacking inter­actions.</div></div><div><div>In the title compound, C₁₆H₉BrO₄, the dihedral angle between the chromen-2-one ring system (r.m.s. deviation = 0.006 Å) and the bromo­benzene ring is 10.29 (6)°. In the crystal, the mol­ecules are connected through C—H⋯O hydrogen bonds and π–π stacking inter­actions. According to a Hirshfeld surface analysis, H⋯H (22.4%), O⋯H/H⋯O (23.6%) and C⋯H/H⋯C (21%) inter­actions are the most significant contributors to the crystal packing.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 200-203"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891593/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603326","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":"Synthesis and crystal structure of 5,10-dihy­droxy-9-meth­oxy-2,2-dimethyl-12-(2-methyl­but-3-en-2-yl)-2H,6H-pyrano[3,2-b]xanthen-6-one","authors":"Amporn Saekee ,&nbsp;Chutima Kuhakarn ,&nbsp;Khetpakorn Chakarawet ,&nbsp;Sakchai Hongthong","doi":"10.1107/S2056989025001070","DOIUrl":"10.1107/S2056989025001070","url":null,"abstract":"<div><div>Methyl­ation of the natural product macluraxanthone yielded its meth­oxy analog, which was characterized by a suite of spectroscopic and crystallographic techniques.</div></div><div><div>5,10-Dihy­droxy-9-meth­oxy-2,2-dimethyl-12-(2-methyl­but-3-en-2-yl)-2<em>H</em>,6<em>H</em>-pyrano[3,2-<em>b</em>]xanthen-6-one, C₂₄H₂₄O₆ (<strong>2</strong>), is a prenylated xanthone that was synthesized from 5,9,10-trihy­droxy-2,2-dimethyl-12-(2-methyl­but-3-en-2-yl)-2<em>H</em>,6<em>H</em>-pyrano[3,2-<em>b</em>]xanthen-6-one or macluraxanthone (<strong>1</strong>), a known compound isolated from <em>Garcinia schomburgkiana</em> Pierre. The present study describes the synthesis of compound <strong>2</strong> by methyl­ation reaction of <strong>1</strong>, and its crystallographic characterization. Compound 2 features a planar xanthone core and a bent pyrano ring adopting a half-boat conformation. An intermolecular O—H⋯O hydrogen bond between the hydroxyl hydrogen donor and the ketone acceptor organizes the molecules into a one-dimensional network along the <em>b</em>-axis direction. Perpendicular to this network, π–π stacking interactions form the three-dimensional supramolecular architecture. These two key intermolecular interactions are distinctly revealed in the Hirshfeld surface analysis.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 219-223"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891587/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603305","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 catena-poly[[[tetra­aquacobalt(II)]-μ2-1,5-di­hydroxy­naphthalene-2,6-di­carboxyl­ato] di­methyl­formamide disolvate]","authors":"Hitoshi Kumagai ,&nbsp;Satoshi Kawata ,&nbsp;Nobuhiro Ogihara","doi":"10.1107/S2056989025000982","DOIUrl":"10.1107/S2056989025000982","url":null,"abstract":"<div><div>The asymmetric unit of the title compound, {[Co(C₁₂H₆O₆)(H₂O)₄]·2C₃H₇NO}_<em>n</em> or {[Co(H₂dondc)(H₂O)₄]·2DMF}_<em>n</em>, comprises half of a Co^II ion, half of a 1,5-di­hydroxy­naphthalene-2,6-di­carboxyl­ate dianion (H₂dondc²⁻), two water mol­ecules and a di­methyl­formamide (DMF) mol­ecule. The key feature of the structure is a three-dimensional hydrogen-bonding network that consists of one-dimensional (1D) coordination chains built up by CoO₆ octa­hedra bridged by H₂dondc²⁻ ligands and inter­chain O–H⋯O hydrogen-bonding inter­actions.</div></div><div><div>The asymmetric unit of the title compound, {[Co(C₁₂H₆O₆)(H₂O)₄]·2C₃H₇NO}_<em>n</em> or {[Co(H₂dondc)(H₂O)₄]·2DMF}_<em>n</em>, comprises half of a Co^II ion, half of a 1,5-di­hydroxy­naphthalene-2,6-di­carboxyl­ate dianion (H₂dondc²⁻), two water mol­ecules and a di­methyl­formamide (DMF) mol­ecule. The Co^II ion, which is located on a crystallographic inversion center, exhibits a distorted six-coord­inated octa­hedral geometry with two oxygen atoms of the H₂dondc²⁻ ligand and four oxygen atoms of the water mol­ecules. The carboxyl­ate group is almost coplanar with the naphthalene moiety and shows monodentate coordination to the Co^II ion. The Co^II ions are bridged by the H₂dondc²⁻ ligand to form a one-dimensional chain. The hy­droxy groups of the ligand have intra-chain hydrogen bonding inter­actions with coordinated water mol­ecules. The coordinated water mol­ecules exhibit not only intra-chain hydrogen bonding inter­actions, but also inter-chain hydrogen-bonding inter­actions. The chains are connected by inter-chain hydrogen-bonding inter­actions and are arranged in parallel to form a two-dimensional network. The chains are further connected by inter-chain hydrogen-bonding inter­actions <em>via</em> the DMF mol­ecules and C—H⋯π inter­actions to give a three-dimensional network.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 204-207"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891581/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603378","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, DFT, mol­ecular docking of 1-[(6-tert-butyl-2-oxo-2H-chromen-4-yl)meth­yl]-4,4-di­methyl­piperidine-2,6-dione and cytotoxic effects on breast cancer (MDA-MB 231), human alveolar basal epithelial (A549) cell lines","authors":"M. Sunitha Kumari ,&nbsp;M. Harish Kumar ,&nbsp;D. V. Deevith ,&nbsp;H. C. Devarajegowda ,&nbsp;B. S. Palakshamurthy","doi":"10.1107/S2056989025001550","DOIUrl":"10.1107/S2056989025001550","url":null,"abstract":"<div><div>The title compound was synthesized by S_N2 reaction of bromo­methyl coumarin with 4,4-di­methyl­piperidine-2,6-dione. Its crystal structure was determined and a Hirshfeld surface analysis was performed along with DFT, mol­ecular docking and biological activity studies.</div></div><div><div>The title compound, C₂₁H₂₅NO₄, was synthesized by S_N2 reaction of bromo­methyl coumarin with 4,4-di­methyl­piperidine-2,6-dione. The mol­ecule crystalizes in the monoclinic system with space group <em>C</em>2/<em>c</em>. The coumarin unit is almost planar with a dihedral angle between the aromatic rings of 0.81 (2)° and an r.m.s deviation of 0.042 Å. The piperidine ring adopts a chair conformation with the two methyl groups, one methyl group occupying an axial position and the other an equatorial position, exhibiting maximum stability. In the crystal, C—H⋯O inter­actions lead to the formation of head-to-head dimers with an <em>R</em>₂²(8)graph-set motif and <em>R</em>₂¹(9) and <em>R</em>₂²(10) ring motifs along [001] and [100]. π–π inter­actions [centroid–centroid distances = 3.885 (2) and 3.744 (2) Å] are also observed. A Hirshfeld surface analysis was carried out, with the two-dimensional fingerprint plots indicating that the major contributions to the crystal packing are from H⋯H(57%), O⋯H(29.3%) and C⋯H(8.1%) inter­actions. The energy framework calculations reveal that dispersion energy (<em>E</em>_dis= −267.7 kJ mol⁻¹) dominates the other energies. The mol­ecular structure was optimized by density functional theory calculations using the B3LYP/6–311+G(d,p) basis set. The HOMO and LOMO orbitals were generated to determine the energy gap, which is 4.245 eV. Mol­ecular docking studies were carried out for the title mol­ecule as ligand and a protein as receptor giving binding affinities of −9.5 kcal mol⁻¹ for PDB ID: 5HG8 and −8.2 kcal mol⁻¹ for PDB ID:6 NLV. The compound was further subjected to biological studies against human cancer cell lines, namely cryopreserved triple negative human breast adenocarcinoma cells (MDA-MB-231cells) and adenocarcinomic human alveolar basal epithelial cells (A549 cells) giving IC₅₀values of 11.57 and 9.34 µ<em>M</em>, respectively. The cytotoxicity results showed a good safety profile against HEK293 cell lines.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 257-263"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891594/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603191","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":"Synthesis, crystal structure, Hirshfeld surface and crystal void analysis of 4-fluoro­benzo[c][1,2,5]selena­diazol-1-ium chloride","authors":"Atash V. Gurbanov ,&nbsp;Tuncer Hökelek ,&nbsp;Gunay Z. Mammadova ,&nbsp;Khudayar I. Hasanov ,&nbsp;Tahir A. Javadzade ,&nbsp;Alebel N. Belay","doi":"10.1107/S2056989025001379","DOIUrl":"10.1107/S2056989025001379","url":null,"abstract":"<div><div>Charge-assisted chalcogen bonds with Se⋯Cl separations of 2.883 (2) and 3.030 (2) Å aggregate the title compound into a supra­molecular dimer.</div></div><div><div>The asymmetric unit of the title salt, C₆H₄FN₂Se⁺·Cl⁻, contains one planar 4-fluoro­benzo[<em>c</em>][1,2,5]selena­diazol-1-ium mol­ecular cation and a chloride anion. In the crystal, inter­molecular N—H⋯Cl hydrogen bonds link the 4-fluoro­benzo[<em>c</em>][1,2,5]selena­diazol-1-ium mol­ecules, which are arranged in parallel layers along (104), to the chloride anions. The cationic layers, in turn, are stacked along [001]. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯Cl/Cl⋯H (22.6%), H⋯F/F⋯H (13.9%), H⋯N/N⋯H (11.9%), H⋯C/C⋯H (10.2%) and H⋯H (7.7%) inter­actions. The volume of the crystal voids and the percentage of free space were calculated to be 44.80 ų and 5.91%, showing that there is no large cavity in the crystal packing.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 252-256"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891591/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603293","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}