Acta Crystallographica Section C Structural Chemistry最新文献

{"title":"Crystal structures and supramolecular and Hirshfeld surface analysis of three novel 2,4,6-triaminopyrimidine salts.","authors":"Marimuthu Mohana, Marimuthu Sangavi, Ray J Butcher","doi":"10.1107/S2053229626007655","DOIUrl":"10.1107/S2053229626007655","url":null,"abstract":"<p><p>Three new hydrous molecular salts, namely, 2,4,6-triaminopyrimidin-1-ium anthranilate (2-aminobenzoate) monohydrate, C₄H₈N₅⁺·C₇H₆NO₂^-·H₂O (I), 2,4,6-triaminopyrimidin-1-ium 5-aminoisophthalate monohydrate, C₄H₈N₅⁺·C₈H₆NO₄^-·H₂O (II), and bis(2,4,6-triaminopyrimidin-1-ium) 4-aminophthalate trihydrate, 2C₄H₈N₅⁺·C₈H₅NO₄^2-·3H₂O (III), have been synthesized and characterized by single-crystal X-ray diffraction techniques. In all three crystal structures, protonation of the pyrimidine moiety occurs at the N1 position and is reflected in a widening of the C-N-C bond angle. In all three cases, protonation of the triaminopyrimidine (TAP) molecule leads to the formation of the robust charge-assisted R₂²(8) TAP-carboxylate heterosynthon, which acts as the primary supramolecular building unit. In salt I, TAP base pairing and water-mediated contacts produce tetrameric aggregates and a DDDA (D is donor and A is acceptor) supramolecular array that propagates into a 3D hydrogen-bonded sheet structure. Salt II exhibits a combination of R₂²(8), R₃²(8) and R₂⁴(8) motifs that fuse to form a continuous hydrogen-bonded chain characterized by a DDDAAA supramolecular array. These chains further assemble into extended sheets which are interconnected by higher-order ring motifs and are reinforced by π-π stacking interactions between the pyrimidine ring and the aromatic anion. The structure of salt III displays the most complex architecture. Multiple hydrogen-bonded arrays, including DADA-type quadruple motifs and large fused-ring motifs, arise through co-operative N-H...O, N-H...N and O-H...O interactions involving the cations, anion and water molecules, resulting in a densely interconnected 3D framework. Hirshfeld surface analysis reveals that H...H contacts dominate the crystal packing, while O...H/H...O and N...H/H...N interactions play a crucial role in directing the supramolecular assembly. The study highlights how anion topology and hydration influence hydrogen-bond hierarchy and supramolecular dimensionality in TAP-based salts.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"513-523"},"PeriodicalIF":1.1,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148676686","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":"Single-crystal structure determination of psilocybin after dehydration.","authors":"Sonya K Emmett, Lee Cameron, Mark Hestermann, Darren Holland, Simon Kessler, Luke McFarlane, Yit Heng Chooi, Stephen A Moggach","doi":"10.1107/S2053229626007692","DOIUrl":"10.1107/S2053229626007692","url":null,"abstract":"<p><p>The crystal structure of the known low-temperature anhydrous phase of psilocybin {3-[2-(dimethylamino)ethyl]-1H-indol-4-yl dihydrogen phosphate, C₁₂H₁₇N₂O₄P} is reported. While the structure was previously characterized using powder X-ray diffraction, this study describes the first determination via single-crystal X-ray diffraction. High-resolution structural models were obtained both before and after in situ dehydration, allowing for a direct comparison of the lattice response to water loss.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"542-546"},"PeriodicalIF":1.1,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13543281/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148688331","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":"Water-bridged tetrameric supramolecular synthons in a novel tetrasubstituted imidazole-phenylalanine derivative synthesized via a Debus-Radziszewski reaction.","authors":"Armando Ferrer, Yonatan Mederos, Santiago V Luis, Ferran Esteve, Belen Altava, América García, Silvio Cunha","doi":"10.1107/S2053229626007321","DOIUrl":"10.1107/S2053229626007321","url":null,"abstract":"<p><p>Leishmaniasis remains a significant global health challenge, as current treatments rely on antimonial compounds that are increasingly limited by toxicity, high costs and emerging drug resistance. In this study, we report the synthesis of a novel 1,2,4,5-tetrasubstituted 1H-imidazole derivative, namely, (2S)-2-[2-(4-nitrophenyl)-4,5-diphenyl-1H-imidazol-1-yl]-3-phenylpropanoic acid monohydrate, C₃₀H₂₃N₃O₄·H₂O, via a Debus-Radziszewski multicomponent reaction using phenylalanine as a chiral precursor. The compound was obtained in 55% yield and its structure was unequivocally characterized by ¹H NMR and FT-IR spectroscopy, and high-resolution mass spectrometry (HRMS). Single-crystal X-ray diffraction analysis revealed an atypical supramolecular architecture defined by a tetrameric synthon. This assembly is orchestrated by two water molecules acting as multidirectional bridges through an intricate hydrogen-bonding network involving the carboxyl groups and pyridinic N atoms. The resulting 3D framework features continuous polar channels and confirms the full retention of the absolute L-configuration of the phenylalanine moiety. These findings highlight the potential of amino acid-functionalized imidazoles as versatile scaffolds for the development of targeted antileishmanial agents.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"588-594"},"PeriodicalIF":1.1,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148808186","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":"Demystifying density functional theory for the crystal engineering community.","authors":"Gregory J O Beran","doi":"10.1107/S2053229626008260","DOIUrl":"10.1107/S2053229626008260","url":null,"abstract":"<p><p>The tutorial on best practices in `0 K' DFT energy calculations on molecular crystal structures by van de Streek & Johnson [Acta Cryst. (2026), C82, 383-400] provides a highly accessible and practical guide for performing reliable periodic density functional theory calculations in organic crystals.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"485-486"},"PeriodicalIF":1.1,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148786854","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":"When the crucible contributes: serendipitous formation, flux reactivity, and crystal and electronic structures of two aluminium-bearing mixed-metal oxides, Ba_2.1Pb_0.9Al_8.8In_2.2O₂₀ and BaAl_1.6Ga_0.4O₄.","authors":"Spencer R Watts, David A Ante, Sviatoslav Baranets","doi":"10.1107/S2053229626008144","DOIUrl":"10.1107/S2053229626008144","url":null,"abstract":"<p><p>Two Al-bearing mixed-metal oxides, Ba_2.11(1)Pb_0.89Al_8.78(1)In_2.22O₂₀, (1), and BaAl_1.57(2)Ga_0.43O₄, (2), were obtained serendipitously from Pb-flux reactions carried out in alumina crucibles. Single-crystal X-ray diffraction analysis determined that (1) crystallizes in the monoclinic space group C2/m [a = 15.9491 (11), b = 11.5929 (8), c = 5.1241 (3) Å and β = 108.644 (2)°] and can be viewed as a disordered derivative of the Pb₃GeAl₁₀O₂₀ structure type. The structure contains mixed octahedrally coordinated Al/In sites and a split Ba/Pb position analogous to the Ba/Bi disorder in Ba₂BiGa₁₁O₂₀. Compound (2) crystallizes in the hexagonal space group P6₃ [a = 9.0981 (3) and c = 8.7909 (4) Å], adopting a superstructure related to the BaAl₂O₄/SrAl₂O₄/BaZnGeO₄ families of oxide materials. Its structure contains mixed Al/Ga tetrahedral sites and positional disorder of bridging O atoms. Electronic structure calculations based on ordered structural models indicate wide-bandgap semiconducting behavior, with a calculated bandgap of 3.63 eV for (1) and 3.80 eV for (2).</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"494-505"},"PeriodicalIF":1.1,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148786913","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":"Peculiarity of atomic displacements in garnets discovered through a single-crystal X-ray diffraction study of the Na-bearing vanadate garnet series.","authors":"Akihiko Nakatsuka, Yuya Miyake, Mami Shimokawa, Kazuake Iishi, Makoto Tokuda, Akira Yoshiasa","doi":"10.1107/S2053229626007217","DOIUrl":"10.1107/S2053229626007217","url":null,"abstract":"<p><p>The structure refinements of the two Na-bearing vanadate garnet series Ca₂NaM₂V₃O₁₂ (M = Co, Ni) and Pb₂NaM₂V₃O₁₂ (M = Mg, Co, Ni) were conducted using single-crystal X-ray diffraction, together with the rerefinements of previously reported Ca₂NaM₂V₃O₁₂ (M = Mg, Mn, Zn, Cd). The crystal chemistry of both vanadate garnet series was discussed with special attention to atomic displacement behaviours, from the combination of the present results with those reported previously for various other garnet compounds. In the investigated compounds, except for Ca₂NaCd₂V₃O₁₂, the dodecahedral-dodecahedral and dodecahedral-octahedral shared edge lengths are unusually longer than or comparable to the corresponding unshared ones, contradicting Pauling's third rule. However, judging from the observation in the Ca₂NaM₂V₃O₁₂ series with a larger number of samples, the ratios of both shared edge lengths to the corresponding unshared ones decrease linearly with increasing octahedral-site cation size. Consequently, in Ca₂NaCd₂V₃O₁₂, with the largest octahedral cation (Cd²⁺) among those investigated here, the dodecahedral-dodecahedral and dodecahedral-octahedral shared edge lengths are significantly shortened compared with the corresponding unshared ones. These observations suggest that the relationships between both shared edge lengths and the corresponding unshared ones respond flexibly to structural geometric constraints depending on the octahedral-site cation size, rather than being subjected to Pauling's third rule. This flexibility results from the insignificant cation-cation repulsions across these shared edges, which are due to the lower mean valence (1.67+) and larger size of the dodecahedral cations than those of previously reported other garnets. In contrast, in all the investigated compounds, including Ca₂NaCd₂V₃O₁₂, the dodecahedral-tetrahedral shared edge lengths are sufficiently shorter than the tetrahedral unshared ones because of the strong repulsion between the dodecahedral and tetrahedral cations brought about by the larger valence of V⁵⁺ at the tetrahedral site. This strong repulsion should result in the smallest mean-square displacements of the tetrahedral cations in the direction of adjacent dodecahedral cations. However, in the Pb₂NaM₂V₃O₁₂ series, the displacements are largest in this direction. This peculiar property is generally observed when the dodecahedral sites are occupied by different cation species with different valences and largely different sizes, as in this series.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"576-587"},"PeriodicalIF":1.1,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148808143","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, structural characterization, and electronic structure of monoclinic α-[SeCl₃][MoOCl₄].","authors":"Thimira Kandabadage, Sherouk M Ibrahim, Sviatoslav Baranets","doi":"10.1107/S2053229626007771","DOIUrl":"10.1107/S2053229626007771","url":null,"abstract":"<p><p>The crystal structure of the monoclinic α-[SeCl₃][MoOCl₄] polymorph, trichloridoselenium tetrachloridooxidomolybdate, is reported from a complete single-crystal X-ray diffraction study. Black-brown moisture-sensitive crystals were obtained from reactions of MoOCl₄ and Se₂Cl₂ in sealed glass ampoules at 100 °C. The compound crystallizes in the space group P2₁/c and is isostructural with the tellurium analog, α-[TeCl₃][MoOCl₄]. Its structure consists of trigonal-pyramidal [SeCl₃]⁺ cations and square-pyramidal [MoOCl₄]^- anions that dimerize through asymmetric Mo...Cl...Mo bridges to form centrosymmetric [Mo₂O₂Cl₈]^2- units. The Se^IV centers exhibit characteristic 3 + 3 coordination, with three short primary Se-Cl bonds and three longer secondary Se...Cl contacts, yielding distorted [SeCl₆] trigonal antiprisms. These contacts connect adjacent [Mo₂O₂Cl₈]^2- dimers into layers parallel to the bc plane. The electronic structure calculations show that α-[SeCl₃][MoOCl₄] has a band gap of ca 0.88 eV. Crystal orbital Hamilton population (COHP) and crystal orbital bond index (COBI) bonding analyses confirm that short primary contacts are covalent, whereas longer secondary Se...Cl and Mo...Cl contacts are significantly weaker yet structurally important for layered connectivity. The natural bond orbital (NBO) analysis further supports charge polarization between the [SeCl₃]⁺ and [MoOCl₄]^- fragments, placing α-[SeCl₃][MoOCl₄] in the realm of layered ionic solids or even van der Waals materials. Bonding of the broad [ChCl₃][MoOCl₄] series (Ch = S, Se, Te) are discussed as well.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"487-493"},"PeriodicalIF":1.1,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148786852","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":"Weak interactions defining the crystal packing in the sterically demanding compound 1-(3-methylphenyl)-2-(4-nitrophenyl)-4,5-diphenyl-1H-imidazole.","authors":"Armando Ferrer, Yonatan Mederos, Julio A Rojas Vargas, Santiago V Luis, Ferran Esteve, Iván Muñoz, Belen Altava, América García","doi":"10.1107/S2053229626005875","DOIUrl":"10.1107/S2053229626005875","url":null,"abstract":"<p><p>The synthesis of 1-(3-methylphenyl)-2-(4-nitrophenyl)-4,5-diphenyl-1H-imidazole, C₂₈H₂₁N₃O₂, has been efficiently achieved in a one-pot procedure from simple materials. Its structure was analysed with the help of a full set of spectroscopic techniques, X-ray crystallographic studies and computational calculations, suggesting that the compound shows some potential for being used in nonlinear optical (NLO) devices. Despite being a sterically demanding tetrasubstituted imidazole, this compound can form a stable crystal structure based on the combination of a large set of weak interactions. With four aryl substituents, displaced and tilted edge-to-face and face-to-face aromatic-aromatic interactions are responsible of many of the short contacts identified, representing the major contribution as determined with the use of Hirshfeld surfaces. The nitro groups also play a key role, being responsible of the polarization of the molecule with the formation of antiparallel assemblies, leading to well-defined stacks. Antiparallel N...O pairs are also present at relatively short distances, together with short H...O contacts (16.9% contribution), indicating the presence of weak hydrogen bonds of the O atoms with weakly acidic H atoms in the polarized structure.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"437-447"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148403208","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":"Best practices in `0 K' DFT energy calculations on molecular crystal structures.","authors":"Jacco van de Streek, Erin R Johnson","doi":"10.1107/S2053229626006169","DOIUrl":"10.1107/S2053229626006169","url":null,"abstract":"<p><p>This article describes best practices for `zero Kelvin' energy calculations on molecular crystals and is targeted for non-experts who would like to perform their own calculations or assess the accuracy and validity of such calculations reported in the scientific literature. The recommended computational procedure can be summarized as follows. (1) Energy optimize the crystal structures of interest with a suitable dispersion-corrected density functional, such as PBE (abbreviated here as PBE+D). (2) Based on the extent of geometric distortions after energy minimization, decide if subsequent energy calculations are required and meaningful. (3) Decide if the PBE+D crystal energies suffice; if they do not, perform a single-point energy calculation on the molecular crystal with a hybrid exchange-correlation functional, such as PBE0, again with a suitable dispersion correction. Similarly, decide if single-point energy calculations on the individual molecules with a more accurate level of theory, such as MP2D or ωB97X+D, are required to improve the molecular energies to account for multiple conformations or tautomers.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"383-400"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13439669/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148403101","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":"Five imide derivatives of 4-azatetracyclo[5.3.2.0^2,6.0^8,10]dodec-11-ene-3,5-dione: hydrogen bonding and intermolecular interactions.","authors":"Taylor Meade, Mitchell Fedewa, Nicolette Owen, Lillie G W Fedewa, Richard J Staples, Shannon M Biros","doi":"10.1107/S2053229626007199","DOIUrl":"10.1107/S2053229626007199","url":null,"abstract":"<p><p>The synthesis, characterization [NMR and low-resolution mass spectrometry (LR-MS)], and X-ray crystal structures of five compounds that contain a 4-azatetracyclo[5.3.2.0^2,6.0^8,10]dodec-11-ene-3,5-dione ring system are reported. The compounds vary in the identity of the substituent on the imide N atom: 2-phenyl, C₁₇H₁₅NO₂ (I); 2-(3-methylphenyl)-, C₁₈H₁₇NO₂ (II); 2-(4-fluorophenyl)-, C₁₇H₁₄FNO₂ (III); 2-(2-fluorophenyl)-, C₁₇H₁₄FNO₂ (IV); and 2-(1-methoxycarbonyl-2-phenylethyl)-, C₂₁H₂₁NO₄ (V). All five compounds feature intermolecular C-H...O hydrogen bonds and the crystals of I-IV also contain C-H...π interactions. The crystals of fluorinated derivatives III and IV both feature C-H...F hydrogen bonds, and compound V is the only crystal to contain intramolecular C-H...O interactions.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"459-467"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148519756","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}