Acta Crystallographica Section E: Crystallographic Communications最新文献

{"title":"Synthesis and structure of (3a<i>RS</i>,10<i>SR</i>,10a<i>SR</i>)-2-(4-chloro-phen-yl)-5-[(4-methyl-phen-yl)sulfon-yl]-1-oxo-1,2,3,3a,4,5,10,10a-octa-hydro-pyrrolo-[3,4-<i>b</i>]carbazole-10-carb-oxy-lic acid with an unknown solvent.","authors":"Elizaveta D Yakovleva, Elena A Sorokina, Victor N Khrustalev, Mehmet Akkurt, Khudayar I Hasanov, Narmina A Guliyeva, Nurlana D Sadikhova, Menberu Mengesha Woldemariam","doi":"10.1107/S2056989026003762","DOIUrl":"https://doi.org/10.1107/S2056989026003762","url":null,"abstract":"<p><p>The title compound, C₂₈H₂₃ClN₂O₅S, crystallizes with two independent mol-ecules (<i>A</i> and <i>B</i>) in the asymmetric unit. In the central fused ring systems, the pyrrolidine rings adopt envelope conformations and the cyclo-hexene rings adopt distorted-half chair conformations. In mol-ecules <i>A</i> and <i>B</i>, the least-squares mean planes of the sixteen-membered central ring systems form dihedral angles of 81.5 (1) and 84.0 (1)°, respectively, with the benzene rings attached to the sulfanyl groups, while they make dihedral angles of 18.6 (1) and 7.7 (1)°, respectively, with the chloro-benzene rings. In the crystal, O-H⋯O hydrogen bonds and weak C-H⋯O and C-H⋯Cl inter-actions link the mol-ecules, forming a three-dimensional network. The contribution of some disordered solvent to the scattering was removed using the SQUEEZE routine [Spek (2015 ▸). <i>Acta Cryst</i>. C71, 9-18] in <i>PLATON</i>. The solvent contribution was not included in the reported mol-ecular weight and density. A Hirshfeld surface analysis indicates that H⋯H (36.8% for mol-ecule <i>A</i>; 29.8% for mol-ecule <i>B</i>), O⋯H/H⋯O (22.1% for <i>A</i> and 27.3% for <i>B</i>), C⋯H/H⋯C (22.1% for <i>A</i> and 20.2% for <i>B</i>) and Cl⋯H/H⋯Cl (9.7% for <i>A</i> and 13.2% for <i>B</i>) inter-actions are the most important contributors to the crystal packing.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"480-484"},"PeriodicalIF":0.6,"publicationDate":"2026-04-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148214/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147832118","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":"Mol-ecular and crystal structure of (1<i>R</i>,3<i>R</i>,4<i>S</i>,7<i>R</i>)-3-bromo-7-(bromo-meth-yl)-1,7-dimethyl-3-nitro-bi-cyclo-[2.2.1]heptan-2-one.","authors":"Vitaliy A Bilenko, Igor V Komarov, Marian V Gorichko, Svitlana V Shishkina","doi":"10.1107/S2056989026003592","DOIUrl":"https://doi.org/10.1107/S2056989026003592","url":null,"abstract":"<p><p>The bicyclic title compound, C₁₀H₁₃Br₂NO₃, is a camphor derivative, crystallizing in the Sohncke space group <i>P</i>2₁2₁2₁, and the absolute configurations of its four chiral C atoms were unambiguously determined. The relative configuration of a bridgehead carbon atom was also confirmed by one- and two-dimensional NMR experiments. In the extended structure, weak C-H⋯O, C-H⋯Br and halogen bonds of the type Br⋯O consolidate the packing.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"473-476"},"PeriodicalIF":0.6,"publicationDate":"2026-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148212/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147831572","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 tetra-aqua-bis-(dimethyl ether)magnesium(II) dibromide dimethyl ether disolvate.","authors":"Beata Moritz, Tristan Mairath, Carsten Strohmann","doi":"10.1107/S205698902600366X","DOIUrl":"https://doi.org/10.1107/S205698902600366X","url":null,"abstract":"<p><p>Unlike typical hexa-hydrates, the title compound, [Mg(C₂H₆O)₂(H₂O)₄]Br₂·2C₂H₆O or [Mg(H₂O)₄(DME)₂]Br₂·DME₂ (DME = dimethyl ether, C₂H₆O), is a water-poor magnesium(II) complex. The central magnesium cation (site symmetry 1) is coordinated by four water mol-ecules and two mol-ecules of dimethyl ether and adopts a slightly elongated <i>trans</i>-octa-hedral coordination geometry. The water mol-ecules are linked to outer-sphere bromide anions and additional dimethyl ether mol-ecules <i>via</i> O-H⋯Br and O-H⋯O hydrogen bonds. Due to the volatility of dimethyl ether, the presence of coordinating and non-coordinating mol-ecules of this ether makes this solid state structure presented here particularly inter-esting. To investigate the inter-molecular inter-actions leading to this special coordination, a Hirshfeld surface analysis was performed. It showed that the H⋯H inter-actions (70.4%) make the largest contribution to the crystal packing, followed by H⋯Br inter-actions (19.4%), H⋯O inter-actions (10.1%) and Br⋯O inter-actions (0.1%).</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"463-466"},"PeriodicalIF":0.6,"publicationDate":"2026-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148208/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147832065","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":"Heterobimetallic Cu-<i>Ln</i> complexes with sulfonyl-amido-phosphate and Schiff base ligands: synthesis and structure.","authors":"Mariia B Struhatska, Viktor O Trush, Olesia V Moroz, Irina S Konovalova, Svitlana V Shishkina, Volodymyr M Amirkhanov","doi":"10.1107/S2056989026003002","DOIUrl":"https://doi.org/10.1107/S2056989026003002","url":null,"abstract":"<p><p>The synthesis and structural characterization of two new heterobimetallic 3<i>d</i>-4<i>f</i> complexes is reported, namely, bis-[dimethyl (phenyl-sulfon-yl)amido-phosphato]-μ-nitrato-(μ-6,6'-{(1<i>E</i>,1'<i>E</i>)-[propane-1,3-diylbis(aza-nylyl-idene)]bis-(methanylyl-idene)}bis-(2-meth-oxy-phenolato))cerium(III)copper(II), [CeCu(C₁₉H₂₀N₂O₄)(C₈H₁₁NO₅PS)₂(NO₃)] or [Cu(Vanpen)Ce(μ-NO₃)(<i>L</i>)₂] (<b>1</b>), and [μ-dimethyl (phenyl-sulfon-yl)amido-phosphato][dimeth-yl(phenyl-sulfon-yl)amido-phosphato](nitrato)(μ-6,6'-{(1<i>E</i>,1'<i>E</i>)-[propane-1,3-diylbis(aza-nylyl-idene)]bis-(methanylyl-idene)}bis-(2-meth-oxy-phenolato))gadolinium(III)copper(II), [CuGd(C₁₉H₂₀N₂O₄)(C₈H₁₁NO₅PS)₂(NO₃)] or [Cu(Vanpen)Gd(μ-<i>L</i>)(<i>L</i>)(NO₃)] (<b>2</b>), obtained by combining the Schiff base (6,6'-{(1<i>E</i>,1'<i>E</i>)-[propane-1,3-diylbis(aza-nylyl-idene)]bis-(methanylyl-idene)}bis-(2-meth-oxy-phenol)) complex Cu(Vanpen) with the lanthanide(III) nitrates and sulfonyl-amido-phosphate (SAPh) ligand dimeth-yl(phenyl-sulfon-yl)amido-phosphate (<i>L</i> ^-). Single-crystal X-ray diffraction studies of Cu-Ce and Cu²⁺-Gd³⁺ complexes reveal that these species contain the <i>Ln</i>(<i>L</i>)₂NO₃ unit. The lanthanide centers adopt nine-coordinate, distorted muffin (<i>Cs</i>) geometries. The coordination modes of <i>L</i> ^- and NO^3- ligands change depending on the lanthanide. In the Cu²⁺-Ce³⁺ complex the NO₃ ^- group acts as a bridging ligand, whereas in the Cu²⁺-Gd³⁺ analogue the bridging function is assumed by SAPh, with NO₃ ^- binding only in a chelating fashion. The presence of a nitrate group can be explained by steric hindrance that prevents coordination of three SAPh ligands around the lanthanide center. Qualitative X-ray fluorescence analysis confirmed the presence of two different metal ions within each heterometallic species.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"467-472"},"PeriodicalIF":0.6,"publicationDate":"2026-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148216/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147832294","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":"Nirmatrelvir methyl <i>tert</i>-butyl ether solvate.","authors":"Jared P Smit, Dale K Purcell, David A Engers, Pamela A Smith, Haley C Bauser, Adrian Radocea","doi":"10.1107/S2056989026003816","DOIUrl":"https://doi.org/10.1107/S2056989026003816","url":null,"abstract":"<p><p>The structure of nirmatrelvir MTBE solvate, C₂₃H₃₂F₃N₅O₄·C₅H₁₂O, at 150 K has monoclinic (<i>P</i>2₁) symmetry. The asymmetric unit contains one nirmatrelvir mol-ecule and one methyl <i>tert</i>-butyl ether solvent mol-ecule. The extended structure consists of N-H⋯O hydrogen bonds that create create [010] chains. Crystals of the title compound were grown from various methyl <i>tert</i>-butyl ether-methanol solvent mixtures, with crystal morphology dependent upon the mixture ratio.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"477-479"},"PeriodicalIF":0.6,"publicationDate":"2026-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148215/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147831840","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 and Hirshfeld surface analysis of 4-(3-hy-droxy-6-meth-oxy-4-oxo-4<i>H</i>-chromen-2-yl)benzaldehyde.","authors":"Arsenii D Snizhko, Viktoriya V Dyakonenko, Eugene S Gladkov, Alexander V Kyrychenko","doi":"10.1107/S2056989026003476","DOIUrl":"https://doi.org/10.1107/S2056989026003476","url":null,"abstract":"<p><p>The asymmetric unit of the title compound, C₁₇H₁₂O₅, contains one crystallographically independent mol-ecule featuring a chromenone fragment with hy-droxy and meth-oxy substituents and a benzaldehyde group. Intra-molecular O-H⋯O, C-H⋯O hydrogen bonds are observed. In the crystal, mol-ecules are linked by O-H⋯O inter-molecular bonds, forming chains along [201]. The Hirshfeld surface analysis shows that the H⋯H and O⋯H/H⋯O contacts dominate the crystal packing with contributions of 34.2% and 27.6%, respectively.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"459-462"},"PeriodicalIF":0.6,"publicationDate":"2026-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148196/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147832341","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":"An analogue of indapamide: crystal structure and Hirshfeld surface analysis of 3-chloro-4-(<i>N</i>,<i>N</i>-diethynylsulfamo-yl)-<i>N</i>-(2-meth-yl-indolin-1-yl)benzamide.","authors":"Youssef Ramli, Wedad Al Garadi, El Mokhtar Essassi, Camille Kalonji Mubengayi, Abdulsalam Alsubari, Joel T Mague","doi":"10.1107/S2056989026003580","DOIUrl":"https://doi.org/10.1107/S2056989026003580","url":null,"abstract":"<p><p>The title mol-ecule, C₂₂H₂₀ClN₃O₃S, adopts a shallow cup-shaped conformation with the chloro-benzamide portion as the bottom. A puckering analysis of the five-membered ring indicates an envelope conformation. In the crystal, helical chains along the <i>a</i>-axis direction are formed by N-H⋯O hydrogen bonds reinforced by C-H⋯π(ring) and weak π-stacking inter-actions. No directed inter-actions between chains appear to exist. A Hirshfeld surface analysis was performed.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"454-458"},"PeriodicalIF":0.6,"publicationDate":"2026-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148209/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147832269","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 and thermal properties of di-aqua-bis-(4-cyano-pyridine)-dithiocyanato-nickel(II).","authors":"Christian Näther","doi":"10.1107/S2056989026003373","DOIUrl":"https://doi.org/10.1107/S2056989026003373","url":null,"abstract":"<p><p>The reaction of Ni(NCS)₂ and 4-cyano-pyridine (C₆H₄N₂) in water leads to the formation of single crystals of the title compound, [Ni(NCS)₂(C₆H₄N₂)₂(H₂O)₂]. The asymmetric unit consists of one Ni^II cation, which is located on a center of inversion, as well as one thio-cyanate anion, one 4-cyano-pyridine coligand and one water mol-ecule in general positions. The nickel cations therefore adopt <i>trans</i>-NiO₂N₄ octa-hedra, forming discrete complexes. These complexes are linked by O-H⋯S hydrogen bonds into layers that lie parallel to the <i>bc</i> plane. These layers are additionally linked by weak C-H⋯N inter-actions into a three-dimensional network. Powder X-ray diffraction (PXRD) indicates that an almost pure sample has been obtained. Upon heating, the title compound loses its water mol-ecules and the 4-cyano-pyridine ligands in separate steps.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"441-445"},"PeriodicalIF":0.6,"publicationDate":"2026-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148219/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147832258","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":"Revisiting symbolic addition: a step-by-step introduction to manual direct methods.","authors":"Thomas E Weirich","doi":"10.1107/S2056989026003300","DOIUrl":"https://doi.org/10.1107/S2056989026003300","url":null,"abstract":"<p><p>Since the mid-1980s, direct methods have become the standard approach for solving crystal structures. However, because the software is now highly automated, the underlying concepts are often less transparent to beginners. This paper therefore revisits the symbolic addition method as a pedagogical framework for understanding phase determination in crystallography. The method is introduced by providing a brief explanation of triplet phase relationships derived from Sayre's equation, as well as their probabilistic interpretation within the formalism of direct methods. This is followed by three fully worked, two-dimensional examples of increasing complexity, which illustrate the method's underlying principles. Starting from subsets of strong, normalized structure factors, the examples describe the complete symbolic addition procedure, including fixing the origin, propagating the phase algebraically through triplet relationships and evaluating trial phase sets using Fourier synthesis. The shown examples provide a transparent, step-by-step demonstration of how phase relationships lead from diffraction intensities to interpretable Fourier maps. Thus, this method and the provided materials can be used as an effective teaching tool to show the principles behind modern, direct methods for determining the atomic structure of crystals.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"534-543"},"PeriodicalIF":0.6,"publicationDate":"2026-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148211/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147831818","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 and Hirshfeld surface analysis of phenyl-methanaminium 2-oxo-2<i>H</i>-chromene-3-carboxyl-ate.","authors":"M Sunithakumari, M U Gagan, V Dwarakanath, H T Srinivasa, H C Devarajegowda, B S Palakshamurthy","doi":"10.1107/S2056989026003403","DOIUrl":"https://doi.org/10.1107/S2056989026003403","url":null,"abstract":"<p><p>The title salt, C₇H₁₀N⁺·C₁₀H₄O^-, formed between 2-oxo-2<i>H</i>-chromene-3-carb-oxy-lic acid and benzyl-amine crystallizes in the triclinic space group <i>P</i>1. Proton transfer from 2-oxo-2<i>H</i>-chromene-3-carb-oxy-lic acid to the NH₂ group of benzyl-amine results in a N-H⋯(O,O) hydrogen bond between cation and the carboxylate group of the anion. The 2-oxo-2<i>H</i>-chromene moiety is almost planar with a dihedral angle between the two fused rings of 1.48 (11)°. The dihedral angle between the rings of the anion and cation is 29.49 (10)°. In the crystal, N-H⋯O hydrogen-bonding inter-actions generate an <i>R</i> ₄ ⁴(12) synthon parallel to the <i>ac</i> plane. The mol-ecules are linked by further C-H⋯π inter-actions, which consolidate the packing. In addition, π-π stacking inter-actions are observed with centroid-to-centroid distances of 3.5832 (14) and 3.8167 (15) Å. The two-dimensional fingerprint plots indicates that the most important contributions to the crystal packing are from H⋯H (39.7%), H⋯O/O⋯H (30.6%) and H⋯C/C⋯H (20.9%) contacts. The anti-bacterial activity, with MIC values of 30 µg ml^-1 against <i>S. aureus</i> and 25 µg ml^-1 against <i>E. coli</i>. The lower MIC against <i>E. coli</i> suggests that the compound is more effective against Gram-negative bacteria than Gram-positive bacteria.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 Pt 5","pages":"432-436"},"PeriodicalIF":0.6,"publicationDate":"2026-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13148198/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147832296","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}