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

{"title":"Magnetic structures in R₅Pt₂In₄ (R = Tb-Tm) investigated by neutron powder diffraction.","authors":"Aleksandra Deptuch, Stanisław Baran, Lukas Keller, Altifani Rizky Hayyu, Andrzej Szytuła","doi":"10.1107/S2052520624004451","DOIUrl":"10.1107/S2052520624004451","url":null,"abstract":"<p><p>Results of the neutron powder diffraction measurements carried out for R₅Pt₂In₄ (R = Tb-Tm) are reported. The compounds crystallize in an orthorhombic crystal structure of the Lu₅Ni₂In₄-type with the rare earth atoms occupying three different sublattices. Neutron diffraction data reveal that at low temperatures the rare earth magnetic moments order below the critical temperature equal to 105, 93, 28, 12 and 3.8 K for R = Tb, Dy, Ho, Er and Tm, respectively. With decreasing temperature the rare earth magnetic moments at the 2a and 4g2 sites order first, while the moments at the 4g1 site order at lower temperatures. Ferrimagnetic order along the c axis, described by the propagation vector k₁ = [0, 0, 0], develops in Tb₅Pt₂In₄ below the Curie temperature (T_C = 105 K). At lower temperatures, an antiferromagnetic component in the ab plane appears. The component is incommensurate with the crystal structure (k₂ = [0, 0.66, ½]), but it turns into a commensurate one (k₃ = [0, 0, ½]) with decreasing temperature. Antiferromagnetic order along the c axis, described by k₄ = [½, 0, 0], is found in Dy₅Pt₂In₄ below the Néel temperature (T_N = 93 K). The k₄-related component disappears below 80 K and the magnetic structure transforms into a ferro/ferrimagnetic one described by k₁ = [0, 0, 0]. Further decrease in temperature leads to the appearance of an incommensurate antiferromagnetic component within the ab plane below 10 K (k₂ = [0, 0.45, ½]), which finally turns into a commensurate one (k₅ = [0, ½, ½]). In Ho₅Pt₂In₄, a sine-modulated magnetic structure with moments parallel to the c axis (k₆ = [⅓,0,0]) is observed below 28 K. With a decrease in temperature, new components, related to k₁ = [0, 0, 0] (bc plane) and k₄ = [½, 0, 0] (c axis), appear. The coexistence of two orderings - in the ab plane (k₁ = [0, 0, 0]) and a modulated one with moments along the b axis (k₇ = [k_x, 0, 0]) - is found in Er₅Pt₂In₄ below 12 K. Decreasing temperature leads to the order-order transformation of the k₁-related component to another one with magnetic moments still constrained to the ab plane and preserved value of the propagation vector (i.e. k₁ = [0, 0, 0]). Tm₅Pt₂In₄ orders antiferromagnetically below T_N = 3.8 K. Thulium magnetic moments lie in the ab plane, while the magnetic structure is described by k₅ = [0, ½ , ½]. The direction of magnetic moments depends on the rare earth element involved and indicates an influence of single ion anisotropy resulting from interaction with the crystalline electric field.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"281-293"},"PeriodicalIF":1.3,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141465514","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":"Supramolecular architectures in multicomponent crystals of imidazole-based drugs and trithiocyanuric acid.","authors":"Anna Ben, Marta Hoelm, Lilianna Chęcińska","doi":"10.1107/S2052520624005055","DOIUrl":"10.1107/S2052520624005055","url":null,"abstract":"<p><p>The structures of three multicomponent crystals formed with imidazole-based drugs, namely metronidazole, ketoconazole and miconazole, in conjunction with trithiocyanuric acid are characterized. Each of the obtained adducts represents a different category of crystalline molecular forms: a cocrystal, a salt and a cocrystal of salt. The structural analysis revealed that in all cases, the N-H...N hydrogen bond is responsible for the formation of acid-base pairs, regardless of whether proton transfer occurs or not, and these molecular pairs are combined to form unique supramolecular motifs by centrosymmetric N-H...S interactions between acid molecules. The complex intermolecular forces acting in characteristic patterns are discussed from the geometric and energetic perspectives, involving Hirshfeld surface analysis, pairwise energy estimation, and natural bond orbital calculations.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"294-304"},"PeriodicalIF":1.3,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11301895/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141490517","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 comparison of the isostructural [Co(NH₃)₅NO₂]XNO₃ and [Co(NH₃)₅ONO]XNO₃, X = Cl^- or Br^- in relation to nitro-nitrito linkage isomerization and photomechanical effects.","authors":"Polina P Kalinina, Alexander S Marchuk, Subash Sahoo, Boris A Zakharov, Elena V Boldyreva","doi":"10.1107/S2052520624002816","DOIUrl":"10.1107/S2052520624002816","url":null,"abstract":"<p><p>A new photoactive cobalt coordination compound, [Co(NH₃)₅NO₂]BrNO₃ (I), was obtained. Its crystal structure was shown to be isostructural with previously known [Co(NH₃)₅NO₂]ClNO₃ (II) for which linkage isomerization accompanied with mechanical response of the crystal has been already reported. Single crystals of I are transformed into nitrito isomer [Co(NH₃)₅ONO]BrNO₃ (III) on irradiation with blue light (λ = 465 nm) without being destroyed. The crystal structure of III was also solved using single-crystal X-ray diffraction and compared with previously known [Co(NH₃)₅ONO]ClNO₃ (IV). A detailed comparison of the structures of I, II, III and IV, including unit-cell parameters, the distribution of free space (in particular, reaction cavities around the nitro ligand), the lengths of hydrogen bonds, coordination and Voronoi-Dirichlet polyhedra has been performed. Single-crystal X-ray diffraction data were complemented with IR spectra. The effect of the replacement of Cl^- by Br^- on the crystal structure and on the nitro-nitrito photoisomerization is discussed.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"171-181"},"PeriodicalIF":1.9,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140854412","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":"Crystal structures of two new high-pressure oxynitrides with composition SnGe₄N₄O₄, from single-crystal electron diffraction.","authors":"Philipp Gollé-Leidreiter, Shrikant Bhat, Leonore Wiehl, Qingbo Wen, Peter Kroll, Ryo Ishikawa, Martin Etter, Robert Farla, Yuichi Ikuhara, Ralf Riedel, Ute Kolb","doi":"10.1107/S2052520624002683","DOIUrl":"10.1107/S2052520624002683","url":null,"abstract":"<p><p>SnGe₄N₄O₄ was synthesized at high pressure (16 and 20 GPa) and high temperature (1200 and 1500°C) in a large-volume press. Powder X-ray diffraction experiments using synchrotron radiation indicate that the derived samples are mixtures of known and unknown phases. However, the powder X-ray diffraction patterns are not sufficient for structural characterization. Transmission electron microscopy studies reveal crystals of several hundreds of nanometres in size with different chemical composition. Among them, crystals of a previously unknown phase with stoichiometry SnGe₄N₄O₄ were detected and investigated using automated diffraction tomography (ADT), a three-dimensional electron diffraction method. Via ADT, the crystal structure could be determined from single nanocrystals in space group P6₃mc, exhibiting a nolanite-type structure. This was confirmed by density functional theory calculations and atomic resolution scanning transmission electron microscopy images. In one of the syntheses runs a rhombohedral 6R polytype of SnGe₄N₄O₄ could be found together with the nolanite-type SnGe₄N₄O₄. The structure of this polymorph was solved as well using ADT.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"182-192"},"PeriodicalIF":1.9,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11157342/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140897039","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":"Supramolecular synthons in hydrates and solvates of lamotrigine: a tool for cocrystal design.","authors":"Gordana Pavlović, Edislav Lekšić, Ernest Meštrović","doi":"10.1107/S2052520624002567","DOIUrl":"10.1107/S2052520624002567","url":null,"abstract":"<p><p>The molecule of anti-epileptic drug lamotrigine [LAM; 3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazine] is capable of the formation of multicomponent solids. Such an enhanced tendency is related to the diverse functionalities of the LAM chemical groups able to form hydrogen bonds. Two robust synthons are recognized in the supramolecular structure of LAM itself formed via N-H...N hydrogen bond: homosynthon, so-called aminopyridine dimer or synthon 1 [R₂²(8)] and larger homosynthon 2 [R₃²(8)]. The synthetic procedures for a new hydrate and 11 solvates of LAM (in the series: with acetone, ethanol: two polymorphs: form I and form II, 2-propanol, n-butanol, tert-butanol, n-pentanol, benzonitrile, acetonitrile, DMSO and dioxane) were performed. The comparative solid state structural analysis of a new hydrate and 11 solvates of LAM has been undertaken in order to establish robustness of the supramolecular synthons 1 and 2 found in the crystal structure of LAM itself as well as LAM susceptibility to build methodical solid state supramolecular architecture in the given competitive surrounding of potential hydrogen bonds. The aminopyridine dimer homosynthon 1 [R₂²(8)] has been switched from para-para (P-P) topology to ortho-ortho (O-O) topology in all crystal structures, except in LAM:n-pentanol:water solvate where it remains P-P. Homosynthon 2 [R₃²(8)] of the LAM crystal structure imitates in the LAM solvates as a heterosynthon by replacing the triazine nitrogen proton acceptor atoms of LAM with the proton acceptors of solvates molecules.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"193-200"},"PeriodicalIF":1.9,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11157341/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140897043","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":"Features of the crystal structure and surface of superprotonic conductor caesium hydrogen sulfate phosphate.","authors":"Irina P Makarova, Natalia N Isakova, Andrey I Kalyukanov, Radmir V Gainutdinov, Alla L Tolstikhina, Vladimir A Komornikov","doi":"10.1107/S2052520624003470","DOIUrl":"10.1107/S2052520624003470","url":null,"abstract":"<p><p>The crystal structure of superprotonic conductor caesium hydrogen sulfate phosphate [Cs₄(HSO₄)₃(H₂PO₄)] have been analyzed using neutron diffraction methods. Additionally, its structure and surface layers have been investigated using atomic force microscopy. From the diffraction data obtained, Fourier syntheses of neutron scattering densities were calculated, and the localization of hydrogen atoms and the parameters of three types of hydrogen bonds in the crystal structure were accurately determined. Correlation of surface characteristics of samples obtained by atomic force microscopy with their crystal structure is shown.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"201-207"},"PeriodicalIF":1.9,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140920178","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":"Ultrasound-assisted synthesis of a Eu³⁺-functionalized Zn^II coordination polymer as a fluorescent dual detection probe for highly sensitive recognition of Hg^II and L-Cys.","authors":"Arash Farahmand Kateshali, Janet Soleimannejad, Jan Janczak","doi":"10.1107/S2052520624003019","DOIUrl":"https://doi.org/10.1107/S2052520624003019","url":null,"abstract":"<p><p>A new Zn^II coordination polymer (CP) based on 2,3-pyrazine dicarboxylic acid (H₂pzdc) and 4,4'-bipyridine (bpy) (ZCP) was synthesized using a facile slow evaporation method. Single-crystal X-ray diffraction revealed that ZCP is a two-dimensional porous CP, [Zn₂(pzdc)₂(bpy)(H₂O)₂]_n, with van der Waals forces as the dominant interaction within its layers forming a 6³ network. Employing energetic ultrasound irradiation, nanoscale ZCP (nZCP) was successfully synthesized and Eu³⁺ ions were incorporated within its host lattice (Eu@nZCP). The resulting platform exhibits superior fluorescence characteristics and demonstrates notable optical durability. Therefore, it was used as a dual detection fluorescent sensing platform for the detection of mercury and L-cysteine (L-Cys) in aqueous media through a turn-off/on strategy. In the turn-off process, the fluorescence emission of Eu@nZCP progressively quenches by the addition of Hg^II via a photo-induced electron transfer (PET) mechanism. The fluorescence of Eu@nZCP is quenched to establish a low fluorescence background through the incorporation of Hg^II. This devised turn-on fluorescent system is suitable for the recognition of L-Cys (based on the strong affinity of L-Cys to the Hg^II ion) through a quencher detachment mechanism. This method attained a relatively wide linear range, spanning from 0.001 to 25 µM, with the low detection limit of 5 nM for the sensing of Hg^II. Also, the corresponding limit of detection (LOD) for L-Cys is 8 nM in a relatively wide linear range, spanning from 0.001 to 40 µM.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":"80 Pt 3","pages":"208-218"},"PeriodicalIF":1.9,"publicationDate":"2024-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141295336","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":"The physical space model of the Tsai-type quasicrystal.","authors":"Ireneusz Buganski, Radoslaw Strzalka, Janusz Wolny","doi":"10.1107/S2052520624000763","DOIUrl":"10.1107/S2052520624000763","url":null,"abstract":"<p><p>The binary Cd_5.7Yb phase representing the Tsai-type category of the icosahedral quasicrystals is solved by the assignment of a unique atomic decoration to rhombohedral units in the Ammann-Kramer-Neri tiling. The unique decoration is found for units with an edge length of 24.1 Å and 3m internal point symmetry. The structural refinement was carried out for two underlying tilings generated by the projection method for 6D space. The difference lies in the location of the origin point which for one tiling is in the vertex and for the second one in the center of the 6D unit cell. The two tilings exhibit mutual duality. The choice of the tiling has a minor effect on the final structural model as both converge to an R factor of ∼11.5%. The main difference is related to the treatment of the Cd4 tetrahedral motif which is either orientationally ordered and aligned with the threefold axis or disordered and modeled as a partially occupied icosahedron. Both models can be presented as a covering by rhombic triacontahedral clusters with identical positions of clusters within rhombohedral units. The shell structure is Tsai-type in the case of the first tiling and Bergman-type for the other.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"84-93"},"PeriodicalIF":1.9,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140027171","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":"Attractive and repulsive forces in a crystal of [Rb(18-crown-6)][SbCl₆] under high pressure.","authors":"Eduard B Rusanov, Michael D Wörle, Maksym V Kovalenko, Kostiantyn V Domasevitch, Julia A Rusanova","doi":"10.1107/S2052520624001586","DOIUrl":"10.1107/S2052520624001586","url":null,"abstract":"<p><p>The compression behavior of [Rb(18-crown-6)][SbCl₆] crystal under pressure up to 2.16 (3) GPa was investigated in a diamond anvil cell (DAC) using a mixture of pentane-isopentane (1:4) as the pressure-transmitting fluid. The compound crystallizes in trigonal space group R3 and no phase transition was observed in the indicated pressure range. The low value of pressure bulk modulus [9.1 (5) GPa] found in this crystal is a characteristic of soft materials with predominant dispersive and electrostatic interaction forces. The nonlinear relationship between unit-cell parameters under high pressure is attributed to the influence of reduced intermolecular H...Cl contacts under pressure over 0.73 GPa. It also explains the high compression efficiency of [Rb(18-crown-6)][SbCl₆] crystals at relatively low pressures, resulting in a significant shift of the Rb atom to the center of the crown ether cavity. At pressures above 0.9 GPa, steric repulsion forces begin to play a remarkable role, since an increasing number of interatomic H...Cl and H...H contacts become shorter than the sum of their van der Waals (vdW) radii. Below 0.9 GPa, both unit-cell parameter dependences (P-a and P-c) exhibit hysteresis upon pressure release, demonstrating their influence on the disordered model of Rb atoms. The void reduction under pressure also demonstrates two linear sections with the inflection point at 0.9 GPa. Compression of the crystal is accompanied by a significant decrease in the volume of the voids, leading to the rapid approach of Rb atoms to the center of the crown ether cavity. For the Rb atom to penetrate into the center of the crown ether cavity in [Rb(18-crown-6)][SbCl₆], it is necessary to apply a pressure of about 2.5 GPa to disrupt the balance of atomic forces in the crystal. This sample serves as a compression model demonstrating the influence of both attractive and repulsive forces on the change in unit-cell parameters under pressure.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"135-145"},"PeriodicalIF":1.9,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10994168/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140183493","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":"Elastic and piezoelectric properties of β-glycine - a quantum crystallography view on intermolecular interactions and a high-pressure phase transition.","authors":"Mark A Khainovsky, Elena V Boldyreva, Vladimir G Tsirelson","doi":"10.1107/S2052520624000428","DOIUrl":"10.1107/S2052520624000428","url":null,"abstract":"<p><p>The effect of hydrostatic compression on the elastic and electronic properties of β-glycine was studied using a quantum crystallography approach. The interrelations between the changes in the microscopic quantum pressure in the electronic continuum, macroscopic compressibility and piezoelectricity were considered. The geometries and energies of hydrogen bonds in the crystal structure of β-glycine were considered as functions of pressure before and after a phase transition into the β'-phase in relation to the mechanism of this phase transition.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":" ","pages":"51-63"},"PeriodicalIF":1.9,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139711180","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}