Acta crystallographica Section B, Structural science, crystal engineering and materials最新文献

{"title":"Quantifying weak interactions in ferroelectric and paraelectric phases of phenazine and chloroanilic acid co-crystal using experimental and theoretical electron densities.","authors":"G N Anil Kumar, Venkatesha R Hathwar","doi":"10.1107/S2052520623007862","DOIUrl":"10.1107/S2052520623007862","url":null,"abstract":"<p><p>The co-crystal of phenazine and chloroanilic acid is known to display paraelectric properties at room temperature. It shows a paraelectric to ferroelectric phase transition at 253 K and has an incommensurately modulated ferroelectric phase below 137 K. High-resolution synchrotron X-ray data were collected at 160 K to model the experimental electron-density distributions, and derived topological properties from the electron density were used to quantify the weak interactions responsible for the origin of the ferroelectric phase. The structure and non-covalent interactions are analysed using Hirshfeld surfaces and energy frameworks. The topological properties, energies, atomic charges and molecular electrostatic potential surfaces are determined from the experimental data, further supported by theoretical calculations. The results from the ferroelectric phase are compared with the paraelectric phase. Although the structural descriptions indicate neutral phenazine and chloroanilic acid molecules in the ferroelectric phase, the topological properties of the electron density indicate a considerable amount of proton transfer in the O-H...O hydrogen bond. Indeed, the displaced H atom in the O-H...O hydrogen bond suggests a mixed covalent/polar nature of chemical bonding. Subtle changes in the chemical bonding and proton-transfer pathways could be detected from the high-resolution electron-density studies.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41107023","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A high-pressure single-crystal X-ray diffraction study of potassium guaninate hydrate, K⁺·C₅H₄N₅O^-·H₂O.","authors":"Anna A Gaydamaka, Sergey V Rashchenko, Anna I Semerikova, Ekaterina S Smirnova, Anna G Ivanova, Sergey G Arkhipov, Boris A Zakharov, Nikita E Bogdanov, Elena V Boldyreva","doi":"10.1107/S2052520623008740","DOIUrl":"10.1107/S2052520623008740","url":null,"abstract":"<p><p>The crystal structure of potassium guaninate hydrate, K⁺·C₅H₄N₅O^-·H₂O, was studied in the pressure range of 1 atm to 7.3 GPa by single-crystal diffraction using synchrotron radiation and a laboratory X-ray diffraction source. Structural strain was compared to that of the same salt hydrate on cooling, and in 2Na⁺·C₅H₃N₅O^2-·7H₂O under hydrostatic compression and on cooling. A polymorphic transition into a new, incommensurately modulated, phase was observed at ∼4-5 GPa. The transition was reversible with a hysteresis: the satellite reflections disappeared on decompression to ∼1.4 GPa.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"71476986","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Order-disorder (OD) polytypism of K₃FeTe₂O₈(OH)₂(H₂O)_1+x.","authors":"Tobias Wolflehner, Berthold Stöger","doi":"10.1107/S2052520623009162","DOIUrl":"10.1107/S2052520623009162","url":null,"abstract":"<p><p>K₃FeTe₂O₈(OH)₂(H₂O)₂ was synthesized under hydrothermal conditions from Te(OH)₆, FeSO₄·7H₂O and 85 wt% KOH in a 1:2:6 molar ratio. The crystal structure is built of a triperiodic network. One disordered water molecule per formula unit is located in a channel and can be partially removed by heating. Systematic one-dimensional diffuse scattering indicates a polytypic character, which is best described by application of the order-disorder theory. The major polytype is monoclinic with pseudo-orthorhombic metrics. It is interrupted by fragments of an orthorhombic polytype. The diffraction intensities are analyzed using structure factor calculations.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833354/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"71476987","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Hydrogen bonding patterns and C-H...π interactions in the structure of the antiparkinsonian drug (R)-rasagiline mesylate determined using laboratory and synchrotron X-ray powder diffraction data.","authors":"Analio J Dugarte-Dugarte, Robert A Toro, Jacco van de Streek, José Antonio Henao, Andrew N Fitch, Catherine Dejoie, José Miguel Delgado, Graciela Díaz de Delgado","doi":"10.1107/S2052520623007758","DOIUrl":"10.1107/S2052520623007758","url":null,"abstract":"<p><p>The structure of (R)-rasagiline mesylate [(R)-RasH⁺·Mes^-], an active pharmaceutical ingredient used to treat Parkinson's disease, is presented. The structure was determined from laboratory and synchrotron powder diffraction data, refined using the Rietveld method, and validated and optimized using dispersion-corrected DFT calculations. The unit-cell parameters obtained in both experiments are in good agreement and the refinement with both datasets converged to good agreement factors. The final parameters obtained from laboratory data were a = 5.4905 (8), b = 6.536 (2), c = 38.953 (3) Å, V = 1398.0 (4) ų and from synchrotron powder data were a = 5.487530 (10) Å, b = 6.528939 (12) Å, c = 38.94313 (9) Å, V = 1395.245 (5) ų with Z = 4 and space group P2₁2₁2₁. Preferred orientation was properly accounted for using the synchrotron radiation data, leading to a March-Dollase parameter of 1.140 (1) instead of the 0.642 (1) value obtained from laboratory data. In the structure, (R)-RasH⁺ moieties form layers parallel to the ab plane connected by mesylate ions through N-H...O and C-H...O hydrogen bonds. These layers stack along the c axis and are further connected by C-H...π interactions. Hirshfeld surface analysis and fingerprint plot calculations indicate that the main interactions are: H...H (50.9%), H...C/C...H (27.1%) and H...O/O...H (21.1%).</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833353/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41187922","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Electron traps and energy storage: modeling a bright path to the future.","authors":"Renaldo T Moura","doi":"10.1107/S205252062301003X","DOIUrl":"10.1107/S205252062301003X","url":null,"abstract":"<p><p>By employing time-dependent density functional theory for solid-state chemistry, the research presented by Andrii Shyichuk [Acta Cryst. (2023), B67, 437-449] significantly contributes to the understanding of electron/hole traps in doped materials.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833356/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138290074","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Design and synthesis of diverse Cd²⁺/Zn²⁺/Cu²⁺ coordination polymers tuned by dicarboxylate and auxiliary 1,4-bis(pyridin-4-ylmethyl)piperazine ligands with luminescence and Hirshfeld surface analyses.","authors":"Nanhao Jin, Yuqi Liu, Siyu Dai, Yanghua Li, Xinying Wang, Yue Zhao, Xiaoming Liu, Han Chen, Huilong Luo, Wei Li","doi":"10.1107/S2052520623007813","DOIUrl":"10.1107/S2052520623007813","url":null,"abstract":"<p><p>Four new coordination polymers, including 1D, 2D and 3D structures, were synthesized via a hydrothermal method using Cd²⁺/Zn²⁺/Cu²⁺ metal salts as nodes. These polymers were formed through self-assembly of four different dicarboxylic acid ligands, namely adamantane-1,3-dicarboxylic acid (H₂adc), glutaric acid (H₂glu), 5-hydroxyisophthalic acid (H₂hip) and fumaric acid (H₂fum), in conjunction with the auxiliary ligand [1,4-bis(pyridin-4-ylmethyl)piperazine (bpmp). The corresponding formulae are [Cd₃(adc)₂(bpmp)Cl₂(H₂O)₂]_n (1), {[Cd₂(glu)₂(bpmp)₂(H₂O)₂]·8H₂O·2CH₃OH}_n (2), [Zn(hip)(bpmp)(H₂O)]_n (3) and [Cu(fum)(bpmp)(H₂O)₂]_n (4). Single-crystal X-ray diffraction studies revealed that the Cd²⁺ centers in complex 1 all adopt a six-coordinate mode but two distinct {CdO₂N₂Cl₂} and {CuO₅Cl} units. The 3D network of complex 1 can be simplified to a binodal (4.6)-connected underlying net with the point symbol (3·4²·5·6²)⁴(3²·6²·7²·8⁸·10). Each Cd²⁺ cation in complex 2 adopts a seven-coordinate {CdO₅N₂} center, forming an asymmetric pentagonal bipyramidal coordination. Its stacking structure is formed by the interaction of hydrogen bonds between 2D supramolecular layers, with the adjacent layers exhibiting mirror symmetry. Each Zn²⁺ ion in complex 3 displays a {ZnO₃N} four-coordinate unit. Its stacking structure is formed by one-dimensional [Zn(hip)(bpmp)(H₂O)]_n chains connected through hydrogen bonds. On the other hand, complex 4 features a Jahn-Teller distorted {CuO₄N₂} octahedral coordination. Subsequently, the thermal stability of these complexes was investigated. The solid-state fluorescence spectroscopy was employed to analyze complexes 1, 2 and 3. Additionally, a Hirshfeld surface analysis was performed on complex 3.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"107589951","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Incommensurate magnetic structure of CrAs at low temperatures and high pressures.","authors":"Andreas Eich, Andrzej Grzechnik, Yixi Su, Bachir Ouladdiaf, Denis Sheptyakov, Thomas Wolf, Vaclav Petricek, Hend Shahed, Karen Friese","doi":"10.1107/S205252062300817X","DOIUrl":"10.1107/S205252062300817X","url":null,"abstract":"<p><p>The magnetic structure of chromium arsenide CrAs is studied with neutron powder diffraction at ambient pressure in the temperature range 1.5-300 K as well as with neutron single-crystal diffraction at 2 K and 0.12 GPa. The material undergoes an anti-isostructural phase transition at T_N = 267 K and atmospheric conditions, in which both orthorhombic phases have the same space-group symmetry (Pnma, Z = 4) but different distortions of the parent hexagonal structure of the NiAs type (P6₃/mmc, Z = 2). The magnetic structure below T_N is incommensurate with the propagation vector k = (0, 0, k_c). At ambient pressure, the component k_c decreases from k_c = 0.3807 (7) at 260 K to k_c = 0.3531 (6) at 50 K. Below this temperature, it is basically constant. With increasing pressure at 2 K, k_c is also constant within standard uncertainties [k_c = 0.353 (2)]. For the analysis of the magnetic structure, a group-theoretical approach based on the space group of the nuclear structure and its subgroups is used. To avoid falling into false minima in the refinements, a random search for magnetic moments in the models is implemented. In the literature, the magnetic structure has been determined on the basis of powder diffraction data as a double helix propagating along the c axis. Although this double-helical model leads to satisfactory agreement factors for our powder data, it does not reproduce the intensities of the magnetic satellite reflections measured on single-crystal data in a satisfactory way and can therefore be discarded. Instead, several other models are found that lead to better agreement. Each of them is spiral-like with directional components in all three directions and with no spin-density wave character that would cause a non-constant magnetic moment. In all these models, the ordering of the spins is neither a pure helix nor a pure cycloid. Instead, the unit vectors of the spin rotation planes make an angle α, 0° < α < 90°, with respect to the c* direction. The model in superspace group P2₁.1'(α0γ)0s yields the best agreement factors in the refinements of the neutron single-crystal and powder diffraction data. This model is unique as it is the only one in which all the magnetic moments rotate with the same chirality.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833358/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41187923","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"3D electron diffraction analysis of a novel, mechanochemically synthesized supramolecular organic framework based on tetrakis-4-(4-pyridyl)phenylmethane.","authors":"Danilo Marchetti, Alessandro Pedrini, Chiara Massera, Moussa Diame Faye Diouf, Christian Jandl, Gunther Steinfeld, Mauro Gemmi","doi":"10.1107/S2052520623007680","DOIUrl":"10.1107/S2052520623007680","url":null,"abstract":"<p><p>Tetrakis-4-(4-pyridyl)phenylmethane (TPPM) is a tetrahedral rigid molecule that crystallizes forming a dynamically responsive supramolecular organic framework (SOF). When exposed to different stimuli, this supramolecular network can reversibly switch from an empty to a filled solvated solid phase. This article describes a novel expanded form of a TPPM-based SOF that has been mechanochemically synthesized and whose crystal structure has been determined by 3D electron diffraction analysis using a novel electron diffractometer.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833357/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41099989","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Ab initio crystal structures and relative phase stabilities for the aleksite series, Pb_nBi₄Te₄S_n+2.","authors":"Jie Yao, Cristiana L Ciobanu, Nigel J Cook, Kathy Ehrig","doi":"10.1107/S2052520623008776","DOIUrl":"10.1107/S2052520623008776","url":null,"abstract":"<p><p>Density functional theory methods are applied to crystal structures and stabilities of phases from the aleksite homologous series, Pb_nBi₄Te₄S_n+2 (n = homologue number). The seven phases investigated correspond to n = 0 (tetradymite), 2 (aleksite-21R and -42R), 4 (saddlebackite-9H and -18H), 6 (unnamed Pb₆Bi₄Te₄S₈), 8 (unnamed Pb₈Bi₄Te₄S₁₀), 10 (hitachiite) and 12 (unnamed Pb₁₂Bi₄Te₄S₁₄). These seven phases correspond to nine single- or double-module structures, each comprising an odd number of atom layers, 5, 7, (5.9), 9, (7.11), 11, 13, 15 and 17, expressed by the formula: S(M_pX_p+1)·L(M_p+1X_p+2), where M = Pb, Bi and X = Te, S, p ≥ 2, and S and L = number of short and long modules, respectively. Relaxed structures show a and c values within 1.5% of experimental data; a and the interlayer distance d_sub decrease with increasing PbS content. Variable Pb-S bond lengths contrast with constant Pb-S bond lengths in galena. All phases are n-fold superstructures of a rhombohedral subcell with c/3 = d_sub*. Electron diffraction patterns show two brightest reflections at the centre of d_sub*, described by the modulation vector q_F = (i/N) · d_sub*, i = S + L. A second modulation vector, q = γ · c_sub*, shows a decrease in γ, from 1.8 to 1.588, across the n = 0 to n = 12 interval. The linear relationship between γ and d_sub allows the prediction of any theoretical phases beyond the studied compositional range. The upper PbS-rich limit of the series is postulated as n = 398 (Pb₃₉₈Bi₄Te₄S₄₀₀), a phase with d_sub (1.726 Å) identical to that of trigonal PbS within experimental error. The aleksite series is a prime example of mixed layer compounds built with accretional homology principles.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833355/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"71419613","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A drug-drug cocrystal and a co-amorphous form, prepared from honokiol and ligustrazine, inspired by Chinese patent medicine.","authors":"Yanli Zhang, Hui Liu, Zongxin Chen, Jialei Meng, Yunfeng Li, Luyao Qi, Suiliang Zhang, Xiaofeng Chen, Ming Lei","doi":"10.1107/S2052520623008648","DOIUrl":"10.1107/S2052520623008648","url":null,"abstract":"<p><p>A drug-drug cocrystal created with two antithrombotic-active ingredients from herbs, honokiol (HON) and ligustrazine (TMP, 1:1), was synthesized and characterized. The structure of HON-TMP (1:1) was determined by single-crystal X-ray diffraction. Then co-amorphous HON-TMP was prepared by honey-assisted grinding, which was inspired by a grinding process for a Chinese patent medicine-Shijunzi honey pill. This co-amorphous drug-drug cocrystal (20% honey) exhibits improved solubility over HON and a significantly reduced sublimation tendency than TMP.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"107589950","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}