Acta Crystallographica Section E: Crystallographic Communications最新文献

{"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 , Peter G. Jones","doi":"10.1107/S2056989025000805","DOIUrl":"10.1107/S2056989025000805","url":null,"abstract":"<div><div>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.</div></div><div><div>The <em>L</em><sub>2</sub><em>MX</em><sub>2</sub> complexes <strong>1</strong>–<strong>5</strong> (<strong>1</strong>: <em>L</em> = <sup><em>t</em></sup>Bu<sup>i</sup>Pr<sub>2</sub>PSe, <em>M</em> = Pd, <em>X</em> = Cl; <strong>2</strong>: <em>L</em> = <sup><em>t</em></sup>Bu<sub>2</sub><sup>i</sup>PrPSe, <em>M</em> = Pd, <em>X</em> = Cl; <strong>3</strong>: <em>L</em> = <sup><em>t</em></sup>Bu<sub>2</sub><sup>i</sup>PrPSe, <em>M</em> = Pd, <em>X</em> = Br; <strong>4</strong>: <em>L</em> = <sup><em>t</em></sup>Bu<sub>2</sub><sup>i</sup>PrPS, <em>M</em> = Pd, <em>X</em> = Br; <strong>5</strong>: <em>L</em> = <sup><em>t</em></sup>Bu<sub>2</sub><sup>i</sup>PrPS, <em>M</em> = Pt, <em>X</em> = Cl) {systematic names: (<em>tert</em>-butyl­diiso­propyl­phosphine selenide-κ<em>Se</em>)di­chlorido­palladium(II), [PdCl<sub>2</sub>(C<sub>10</sub>H<sub>23</sub>PSe)<sub>2</sub>] (<strong>1</strong>), (di-<em>tert</em>-butyl­iso­propyl­phosphine selenide-κ<em>Se</em>)di­chloridopalladium(II), [PdCl<sub>2</sub>(C<sub>11</sub>H<sub>25</sub>PSe)<sub>2</sub>] (<strong>2</strong>), di­bromido­(di-<em>tert</em>-butyl­iso­propyl­phosphine selenide-κ<em>Se</em>)palladium(II), [PdBr<sub>2</sub>(C<sub>11</sub>H<sub>25</sub>PSe)<sub>2</sub>] (<strong>3</strong>), di­bromido­(di-<em>tert</em>-butyl­iso­propyl­phosphine sulfide-κ<em>S</em>)palladium(II), [PdBr<sub>2</sub>(C<sub>11</sub>H<sub>25</sub>PS)<sub>2</sub>] (<strong>4</strong>), di­chlorido­(di-<em>tert</em>-butyl­iso­propyl­phosphine sulfide-κ<em>S</em>)palladium(II), [PdCl<sub>2</sub>(C<sub>11</sub>H<sub>25</sub>PS)<sub>2</sub>] (<strong>5</strong>)} all display a <em>trans</em> configuration with square-planar geometry at the metal atom. Compounds <strong>2</strong> and <strong>3</strong> are isotypic. The mol­ecules of <strong>1</strong> and <strong>4</strong> display crystallographic inversion symmetry; compound <strong>5</strong> 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 <strong>6</strong>, (<sup><em>t</em></sup>Bu<sup>i</sup>Pr<sub>2</sub>PS)<sub>2</sub>Pd<sub>2</sub>Cl<sub>4</sub> {systematic name: di-μ-chlorido-bis­[(<em>tert</em>-butyldiiso­propyl­phosphine sulfide-κ<em>S</em>)chlorido­palladium(II)], [PdCl<sub>2</sub>(C<sub>10</sub>H<sub>23</sub>PS)<sub>2</sub>]}, is dinuclear with a central Pd<sub>2</sub>Cl<sub>2</sub> 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}

{"title":"Synthesis and crystal structures of five fluorinated diphenidine derivatives","authors":"Ryan E. Mewis ,&nbsp;Matthew C. Hulme ,&nbsp;Jack Marron ,&nbsp;Stuart K. Langley ,&nbsp;Oliver B. Sutcliffe ,&nbsp;Sophie L. Benjamin","doi":"10.1107/S2056989025001288","DOIUrl":"10.1107/S2056989025001288","url":null,"abstract":"<div><div>The crystal structures of five fluorinated diphenidine mol­ecules obtained as their hydro­chloride salts are reported.</div></div><div><div>Diphenidine (<strong>1a</strong>), a dissociative anaesthetic, was first reported in 2013. Since then, a number of derivatives <em>e.g.</em> 2-methoxphenidine (<strong>1b</strong>) have been produced by clandestine laboratories and sold as <em>research chemicals</em>. Fluorinated diphenidines, namely, [1-(2,6-di­fluoro­phen­yl)-2-phenyl­eth­yl]di­methyl­aza­nium chloride, C₁₆H₁₈F₂N⁺·Cl⁻, (<strong>I</strong>), [1-(2,6-di­fluoro­phen­yl)-2-phenyl­eth­yl](eth­yl)aza­nium chloride di­chloro­methane hemisolvate, 2C₁₆H₁₈F₂N⁺·2Cl⁻·CH₂Cl₂, (<strong>II</strong>), <em>tert</em>-but­yl[1-(2,6-di­fluoro­phen­yl)-2-phenyl­eth­yl]aza­nium chloride, C₁₈H₂₂F₂N⁺·Cl⁻, (<strong>III</strong>), 1-[1-(2,6-di­fluoro­phen­yl)-2-phenyl­eth­yl]pyrrolidin-1-ium chloride, C₁₈H₂₀F₂N⁺·Cl⁻, (<strong>IV</strong>), and 1-[1-(2,3,4,5,6-penta­fluoro­phen­yl)-2-phenyl­eth­yl]piperidin-1-ium chloride, C₁₉H₁₉F₅N⁺·Cl⁻, (<strong>V</strong>), were synthesized and structurally characterized by ¹H, ¹³C and ¹⁹F NMR spectroscopy, and single-crystal X-ray diffraction. All five structures exhibit hydrogen bonding between the quaternary amine hydrogen atoms and the chlorine. The N—H⋯Cl distances for (<strong>II</strong>) and (<strong>III</strong>) range from 2.21 to 2.31 Å, whereas (<strong>I</strong>), (<strong>IV</strong>) and (<strong>V</strong>) exhibit shorter N—H⋯Cl distances (2.07–2.20 Å). Compounds (<strong>IV</strong>) and (<strong>V</strong>) include pyrrolidine and piperidine rings, respectively; the pyrrolidine ring adopts an envelope conformation whereas the piperidine ring adopts a chair conformation. The crystal packing in compounds (<strong>I</strong>)–(<strong>V</strong>) is characterized by C—H⋯π inter­actions; no π–π inter­actions are observed.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 3","pages":"Pages 229-234"},"PeriodicalIF":0.5,"publicationDate":"2025-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11891590/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143603319","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}