Acta Crystallographica Section C Structural Chemistry最新文献

{"title":"Nucleophilic substitution of a phthalimidyl group with morpholine in an N¹-methyl-1,2,3-triazole: crystallographic evidence for migration of the methylene bridge.","authors":"Paul R Palme, Richard Goddard, Markus Leutzsch, Adrian Richter, Peter Imming, Rüdiger W Seidel","doi":"10.1107/S2053229626002810","DOIUrl":"10.1107/S2053229626002810","url":null,"abstract":"<p><p>2-{[4-(4-Bromophenyl)-1H-1,2,3-triazol-1-yl]methyl}phthalimide, C₁₇H₁₁BrN₄O, was synthesized by click chemistry employing a copper-catalyzed azide-alkyne 1,3-dipolar cycloaddition. The molecule adopts an angular structure and was found to crystallize in the monoclinic system (space group P2₁/n, Z = 4). Reaction with morpholine in the presence of a base afforded 4-{[4-(4-bromophenyl)-2H-1,2,3-triazol-2-yl]methyl}morpholine, C₁₃H₁₅BrN₄O, as the major product, involving a nucleophilic substitution of morpholine for the phthalimide group and migration of the substituent from N1 to N2 on the 1,2,3-triazole ring. The morpholine-substituted compound likewise crystallizes in the monoclinic system (space group P2₁/c, Z = 4) with the molecule exhibiting an angular shape. Both crystal structures appear to be governed by close packing, with weak C-H...O and C-H...N hydrogen bonds as the prevailing intermolecular interactions.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"144-150"},"PeriodicalIF":0.9,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13051533/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147508722","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A case study of the inflexible bis-hydrazone butane-2,3-dione bis[(fluoren-9-ylidene)hydrazone].","authors":"Vikrant Jayant, Shakeel Alvi, Lubna Khan, Mohd Tauqeer, Rashid Ali","doi":"10.1107/S2053229626002706","DOIUrl":"10.1107/S2053229626002706","url":null,"abstract":"<p><p>The crystal structure of the fluorenone-based bis-hydrazone butane-2,3-dione bis[(fluoren-9-ylidene)hydrazone], C₃₀H₂₂N₄, consists of two fluorene subunits connected by a conjugated =N-N=C-C=N-N= chain. The compound was synthesized by condensation between fluorenone and hydrazine in acetic acid. Although the molecule contains bulky fluorenyl moieties on the termini of the conjugated chain, no polymorphs or solvated phases were obtained. Two methyl groups were found to be located in trans positions with respect to one another, thereby providing extra stability to the rigid bis-hydrazone.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"189-198"},"PeriodicalIF":0.9,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147571356","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Hydrogen-bonding functionalities of selected azole drugs in multicomponent crystals with trithiocyanuric acid.","authors":"Anna Ben, Małgorzata Domagała, Lilianna Chęcińska","doi":"10.1107/S2053229626003219","DOIUrl":"10.1107/S2053229626003219","url":null,"abstract":"<p><p>Five new multicomponent crystalline forms of trithiocyanuric acid with azole active pharmaceutical ingredients (APIs) are described. The azole APIs include imidazole-derived econazole and luliconazole, as well as 1,2,4-triazole-derived isavuconazole, voriconazole and posaconazole, and the crystalline forms reported are econazolium trithiocyanurate, C₁₈H₁₆Cl₃N₂O⁺·C₃H₂N₃S₃^-, luliconazole-trithiocyanuric acid (1/1), C₁₄H₉Cl₂N₃S₂·C₃H₃N₃S₃, isavuconazole-trithiocyanuric acid (1/1), C₂₂H₁₇F₂N₅OS·C₃H₃N₃S₃, voriconazole-trithiocyanuric acid-water (1/2/3), C₁₆H₁₄F₃N₅O·2C₃H₃N₃S₃·3H₂O, and posaconazole-trithiocyanuric acid (1/1), C₃₇H₄₂F₂N₈O₄·C₃H₃N₃S₃. The crystal architectures are analyzed in the context of the supramolecular assemblies they generate. Robust acid-base pairs, governed by N-H...N hydrogen bonds, are combined into well-defined four-molecule assemblies through N-H...S hydrogen bonds, which form the characteristic ring R²₂(8) synthon between two TTCA molecules. Additional N-H...O or N-H...S interactions, involving the remaining azole functionalities, propagate these four-molecule units into extended chain motifs, columns or layered architectures. To elucidate the nature of these key interactions, a QTAIM analysis was performed and pairwise interaction energies were evaluated to clarify the stability and energetics of the resulting assemblies. The influence of chiral azole molecules, their specific hydrogen-bond functionalities and the solvation conditions on the formation of the supramolecular motifs is also discussed.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"176-188"},"PeriodicalIF":0.9,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147525362","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Structure and optical properties of a trimetallic cobalt-molybdenum-sodium metal-organic framework.","authors":"Benjamin J Moore, Jeremiah P Tidey, Craig I Hiley, Richard I Walton","doi":"10.1107/S205322962600077X","DOIUrl":"10.1107/S205322962600077X","url":null,"abstract":"<p><p>The crystallization of a trimetallic cobalt-molybdenum-sodium metal-organic <!?tlsb=-0.05pt>framework, poly[μ-benzene-1,3,5-tricarboxylato-tetra-μ-oxido-cobaltmolybdenumtrisodium], UOW-10 or [Na₃Co(MoO₄)(BTC)]_n, is achieved by solvothermal synthesis using benzene-1,3,5-tricarboxylic acid (H₃BTC, C₉H₆O₆) as a ligand precursor, Na₂MoO₄·2H₂O and Co(NO₃)₂·2H₂O as metal sources, and N,N-dimethylformamide (DMF) as the solvent. 3D electron diffraction (3D ED) reveals that the structure crystallizes in the monoclinic space group P2₁/c, with lattice parameters of a = 9.718 (2), b = 18.250 (3), c = 6.892 (9) Å, α = γ = 90, β = 96.156 (15)°, V = 1214.7 (4) ų and Z = 4. The phase purity of the bulk sample was confirmed using synchrotron powder X-ray diffraction. The organic ligands form a 2D layer, where cobalt and molybdenum are found, with sodium cations located between the layers. There are four crystallographically distinct sodium sites: three exhibit a distorted octahedral coordination geometry, while the remaining site is seven-coordinate. The cobalt has trigonal bipyramidal coordination geometry and molybdenum exhibits a tetrahedral coordination geometry. Half the sodium cations in the structure forms 1D column-like motifs via shared oxygen edges along the crystallographic c axis, which are cross-linked in b by the cobalt and molybdenum sites via bridging O atoms, while the other half of the sodium cations form 2D ribbons in the ac plane, propagating along c, linked by sharing oxygen edges and faces. The optical properties of UOW-10 were investigated through the use of UV-Vis spectroscopy, showing a bandgap of 1.8 eV. Deconvolution of the features in the visible-light region reveals that four peaks are present, which can all be ascribed to the d-d transitions from the trigonal bipyramidal cobalt. By means of thermogravimetric analysis (TGA) and variable-temperature powder X-ray diffraction (VT-PXRD), it is demonstrated that the material has thermal stability to 410 °C, after which structure collapse occurs, leading to a mixture of Na₂MoO₄, CoO and Co₃Mo above 900 °C.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"102-109"},"PeriodicalIF":0.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12961748/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146148694","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Salt forms of a thioamide: protonation of 1-(2,6-dimethylphenyl)thiourea.","authors":"Kristin Donnachie, Bethany Gibson, Alan R Kennedy, Connor MacCall, Marc Reid","doi":"10.1107/S2053229626001804","DOIUrl":"10.1107/S2053229626001804","url":null,"abstract":"<p><p>Treating the thioamide 1-(2,6-dimethylphenyl)thiourea (C₉H₁₂N₂S, DMPT) with concentrated aqueous strong acids gave three salt forms with protonation at the thioamide S atom. The structures of 1-(2,6-dimethylphenyl)thiouronium chloride, C₉H₁₃N₂S⁺·Cl^- or [DMPT(H)][Cl], 1-(2,6-dimethylphenyl)thiouronium bromide, C₉H₁₃N₂S⁺·Br^- or [DMPT(H)][Br], and 1-(2,6-dimethylphenyl)thiouronium hydrogen sulfate, C₉H₁₃N₂S⁺·HSO₄^- or [DMPT(H)][HSO₄], are compared with that of neutral DMPT. Protonation at the S atom results in a systematic lengthening of the C=S bond and a shortening of the C-N bonds, with a larger effect found for the bonds involving the secondary amine rather than the primary amine function. The [DMPT(H)]⁺ cations are found to adopt one of two possible conformations, with the halide species having secondary N-H syn to S-H, whilst in the hydrogen sulfate structure, this relationship is anti. The change in cation conformation is related to a change in the hydrogen-bonding motif, but all three salt forms form layered structures with two-dimensional hydrogen-bonded units separated by layers of hydrophobic arene rings. An alternative product type was isolated on adding DMPT to concentrated sulfuric or tetrafluoroboric acid. Structures of the dicarbocationic disulfide species (disulfane-1,2-diyl)bis[N-(2,6-dimethylphenyl)methanediaminium] bis(tetrafluoroborate), C₁₈H₂₄N₄S₂²⁺·2BF₄^- or [Dimer][BF₄]₂, and (disulfane-1,2-diyl)bis[N-(2,6-dimethylphenyl)methanediaminium] bis(hydrogen sulfate) monohydrate, C₁₈H₂₄N₄S₂²⁺·2HSO₄^-·H₂O or [Dimer][HSO₄]₂·H₂O, are also described.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"129-137"},"PeriodicalIF":0.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12961746/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147281719","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Effect of counteranions on the crystal structures of Zn^II coordination polymers with 1,3-bis(1H-imidazol-1-yl)benzene.","authors":"Sidan Geng, Jiayi Jiang, Jingui Duan","doi":"10.1107/S205322962600152X","DOIUrl":"10.1107/S205322962600152X","url":null,"abstract":"<p><p>Two new coordination compounds, catena-poly[[[diaquazinc(II)]-bis[μ-1,3-bis(1H-imidazol-1-yl)benzene]] bis(tetrafluoroborate)], {[Zn(C₁₂H₁₀N₄)₂(H₂O)₂](BF₄)₂}_n, 1, and catena-poly[[[diaquazinc(II)]-bis[μ-1,3-bis(1H-imidazol-1-yl)benzene]] hexafluorotitanate], {[Zn(C₁₂H₁₀N₄)₂(H₂O)₂][TiF₆]}_n, 2, have been synthesized and structurally characterized. Both compounds exhibit analogous cationic 1D coordination chains, {[Zn(L)₂(H₂O)₂]²⁺}_n, where L is 1,3-bis(1H-imidazol-1-yl)benzene. However, the identity of the counteranion, i.e. BF₄^- in 1 and [TiF₆]^2- in 2, significantly influences the supramolecular architecture and porosity due to differences in size, geometry and charge. In 1, the small monovalent BF₄^- anion stabilizes an extended conformation of the ligand and occupies channels without causing disruption, facilitating the assembly of a nonporous supramolecular framework through hydrogen-bonding interactions. Conversely, the larger [TiF₆]^2- dianion in 2 induces a more compact conformation of the ligand, occupies potential pore spaces and promotes inter-chain hydrogen bonds, resulting in a dense layered structure. However, the face-to-face packing of these layers creates an open porous architecture. This study highlights the role of anions as templates in modulating hierarchical assembly, ligand conformation and the resultant porosity in coordination polymers.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"110-115"},"PeriodicalIF":0.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146256957","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Room-temperature crystal structures of [CH(NH₂)₂]₃Sb₂X₉ (X = Br and I).","authors":"Prajna Bhatt, Yuhan Liu, Anna Regoutz, Robert G Palgrave","doi":"10.1107/S2053229626000811","DOIUrl":"10.1107/S2053229626000811","url":null,"abstract":"<p><p>Crystals of formamidinium antimony, halides, FA₃Sb₂X₉ {FA = [CH(NH₂)₂]⁺; X = Br^- and I^-} {or triformamidinium nonahalidodiantimony, (CH₅N₂)₃[Sb₂X₉]}, have been synthesized using a counter diffusion crystal growth (CDCG) method in silica gel and their structures determined from single-crystal X-ray diffraction data. FA₃Sb₂Br₉ belongs to the trigonal space group P3m1, which is known as the Cs₃Bi₂Br₉ structure type, and FA₃Sb₂I₉ belongs to the hexagonal space group P6₃/mmc, called the Cs₃Cr₂Cl₉ structure type. The change of the anion type from bromide to iodide results in the change of the structure type and the connectivity of the Sb-X octahedra. These structures are described and compared to the crystal types known for vacancy-ordered triple-perovskites.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"138-143"},"PeriodicalIF":0.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12961747/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147289123","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Structural and biological aspects of (tert-butoxycarbonylamino)propylphosphonate derivatives.","authors":"Andrzej Olczak, Aleksandra Trocha, Iwona E Głowacka, Dorota G Piotrowska, Izabela Korona-Głowniak, Katarzyna Suśniak, Marcin Zaborowski, Małgorzata Szczesio","doi":"10.1107/S2053229626001440","DOIUrl":"10.1107/S2053229626001440","url":null,"abstract":"<p><p>A promising trend in the search for new more effective and selective drugs is the search for structural analogues of amino acids. The structures and activities of both enantiomeric diethyl (1S,2R)- and (1R,2S)-1,2-bis(tert-butoxycarbonylamino)propylphosphonates (as the monohydrates, C₁₇H₃₅N₂O₇P·H₂O), 1 and 2, respectively, and racemic diethyl (RS)-2-(tert-butoxycarbonylamino)propylphosphonate, 3, have been determined. The antimicrobial activity of 1, 2 and 3 was tested against reference bacterial strains and showed weak bioactivity against Gram-positive bacteria. ADME (absorption, distribution, metabolism and excretion) analysis indicates that the compounds may have gastrointestinal absorption. The compounds satisfy Lipinski's rules.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"116-122"},"PeriodicalIF":0.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146256955","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Chiral three-dimensional cadmium(II)-based coordination polymer constructed from a lactic acid derivative: synthesis, structure and properties.","authors":"Xiu Ju Yin, Yan Lin, Jia Hui Luo, Xiao Ling Wang, Yuan Lu, Zhong Xuan Xu","doi":"10.1107/S2053229626001671","DOIUrl":"10.1107/S2053229626001671","url":null,"abstract":"<p><p>To obtain coordination polymers with nonlinear optical (NLO) activity, the lactic acid derivative (R)-5-(1-carboxyethoxy)isophthalic acid, or (R)-H₃cia, was selected as the chiral ligand. Through a solvothermal reaction with Cd²⁺ in the presence of pyrazine (pyr), the chiral complex poly[tetraaquabis[μ-(R)-5-(1-carboxylatoethoxy)isophthalato](μ-pyrazine)tricadmium(II)], {[Cd₃(C₁₁H₇O₇)₂(C₄H₄N₂)(H₂O)₄]_n or [Cd₃{(R)-cia}₂(pyr)(H₂O)₄]_n (abbreviated as HU32-R), was synthesized successfully. Single-crystal X-ray diffraction analysis reveals that HU32-R crystallizes in the monoclinic space group I2 and features a three-dimensional framework. The complex exhibits good phase purity and certain water stability. Solid-state circular dichroism (CD) spectroscopy confirms its macroscopic chirality. Fluorescence spectroscopy shows an emission peak at 487 nm upon excitation at 365 nm. Furthermore, second-harmonic generation (SHG) measurements indicate that HU32-R possesses significant second-order NLO activity, with an intensity approximately 0.72 times that of potassium dihydrogen phosphate (KDP).</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"123-128"},"PeriodicalIF":0.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147269406","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis, structure and characterization of a new glycolate: sodium glycolate-glycolic acid (1/1).","authors":"Mingyang Hu, Bin Lian","doi":"10.1107/S2053229625011635","DOIUrl":"10.1107/S2053229625011635","url":null,"abstract":"<p><p>Among various glycolates, potassium glycolate glycolic acid (PGGA), ammonium glycolate glycolic acid (AGGA) and rubidium glycolate glycolic acid (RGGA) are isostructural, with the general formula A(C₂H₃O₃)(C₂H₄O₃) (A = K, NH₄ and Rb). However, whether Na⁺ can occupy the A site and its effects on structure and properties remained unknown. This study synthesized sodium glycolate glycolic acid (SGGA), analyzed its composition, structure, vibrational spectra and thermal behaviour, and compared the results with PGGA. SGGA has the formula Na⁺·C₂H₃O₃^-·C₂H₄O₃ or Na(C₂H₃O₃)(C₂H₄O₃), with orthorhombic crystallinity. Although the salt lacks chiral C atoms, it crystallizes in the unique chiral space group P2₁2₁2₁. Among various glycolates, only PGGA and RGGA display relatively similar powder X-ray diffraction (PXRD) patterns, while those of other glycolates are distinctly different, providing a key basis for distinguishing A(C₂H₃O₃)(C₂H₄O₃) glycolates. Although SGGA and PGGA show closely related vibrational spectra and thermal behaviour due to structural similarities, differences are observed in certain spectral peaks. Moreover, PGGA decomposes into carbonates at a marginally higher temperature than SGGA. This work provides insight into glycolic acid bonding and the structural role of Na⁺ in glycolates, guiding new mineral discovery.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"60-67"},"PeriodicalIF":0.9,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145931781","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}