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

{"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":null,"pages":null},"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":null,"pages":null},"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":null,"pages":null},"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":null,"pages":null},"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":"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":null,"pages":null},"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}

{"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":null,"pages":null},"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":"Effect of a halogen bond on the crystal structure of terphenyldicarboxylic acid derivatives.","authors":"Artyom A Osipov, Sergey A Nayfert, Sergey A Sobalev, Kanthapazham Rajakumar, Dmitry A Zherebtsov, Dar'ya V Spiridonova, Denis A Vinnik","doi":"10.1107/S2052520624001318","DOIUrl":"10.1107/S2052520624001318","url":null,"abstract":"<p><p>The syntheses and structures of dimethyl [1¹,2¹:2⁴,3¹-terphenyl]-1⁴,3⁴-dicarboxylate (1), dimethyl 2²,2⁵-diiodo[1¹,2¹:2⁴,3¹-terphenyl]-1⁴,3⁴-dicarboxylate (2), potassium [1¹,2¹:2⁴,3¹-terphenyl]-1⁴,3⁴-dicarboxylate (3) and dimethyl [1,1'-biphenyl]-4,4'-dicarboxylate (4) are reported. Neighboring phenyl rings in compounds 1, 3 and 4 have a planar structure (torsion angles are 0.6-4.1°) and the molecules are packed into regular layers. In the structure of the iodinated derivative of terphenyldicarboxylic acid (2), the middle benzene ring of the terphenyl fragment is rotated relative to the other rings by 64° due to the repulsion between the protons and the iodine atoms of neighboring rings. The formation of halogen bonds between iodine and oxygen atoms of the carbonyl group leads to the movement of molecules of one layer into another layer and the loss of layered structure. Potassium [1¹,2¹:2⁴,3¹-terphenyl]-1⁴,3⁴-dicarboxylate (3) forms crystals with an ionic structure. The coordination number of the potassium cation is eight and the resulting coordination polyhedron is a distorted square antiprism. Dianions in the potassium salt crystal are packed in layers similar to the layers in the dimethyl ethers 1 and 4. Salt 3 has high thermal stability to 500°C.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140183515","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":"Growth, crystal structure and IR luminescence of KSrY_1-xEr_x(BO₃)₂.","authors":"Artem B Kuznetsov, Konstantin A Kokh, Liudmila A Gorelova, Dmitry O Sofich, Nursultan Sagatov, Pavel N Gavryushkin, Oleg S Vereshchagin, Vladimir N Bocharov, Vyacheslav S Shevchenko, Alexander E Kokh","doi":"10.1107/S205252062400177X","DOIUrl":"10.1107/S205252062400177X","url":null,"abstract":"<p><p>A series of novel KSrY_1-xEr_x(BO₃)₂ (x = 0-1) phosphors that emit near-infrared radiation was synthesized using solid-state methods. Pure Y and Er crystals were grown using a KF flux via the top-seeded solution growth technique. In situ high-temperature single crystal X-ray diffraction, Raman spectroscopy and DFT calculations were used for characterization. Within the series, a polymorphic phase transition from space group P2₁/m to R3m was discovered between 550 and 600°C. The concentration dependence of the luminescence intensity was measured for the samples. A strong emission of Er³⁺ electron transition ⁴I_13/2 → ⁴I_15/2 was detected within the 1529-1549 nm range, with the maximum observed for the KSrY_0.4Er_0.6(BO₃)₂ composition.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140183516","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":"Structural changes in Rochelle salt on phase transitions revisited in a multi-temperature single-crystal X-ray diffraction study.","authors":"Svetlana S Sharaya, Boris A Zakharov, Elena V Boldyreva","doi":"10.1107/S205252062400115X","DOIUrl":"10.1107/S205252062400115X","url":null,"abstract":"<p><p>Phase transitions in Rochelle salt [sodium potassium L(+)-tartrate tetrahydrate] are revisited in a single-crystal X-ray diffraction multi-temperature study on cooling from 308 to 100 K across the high-temperature paraelectric (PE) ↔ ferroelectric ↔ low-temperature PE phase transition points. The results of structure refinement using three different models (a harmonic with and without disorder, and an anharmonic) were compared. The temperature dependencies of anisotropic displacement parameters (ADPs) and U_eq, which can be calculated directly from ADPs, for the low-temperature PE phase indicate clearly the dynamic nature of disorder of the K1 atoms. The structures of the low-temperature and the high-temperature PE phases are compared for the first time at multiple temperatures for each phase based on diffraction data collected from the same single crystal. The data indicate that the high-temperature and the low-temperature paraelectric phases are probably not two different phases, as was assumed in earlier works, but are structurally the same phase at different temperatures.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140027170","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 structure solution and high-temperature thermal expansion in NaZr₂(PO₄)₃-type materials.","authors":"Benjamin S Hulbert, Julia E Brodecki, Waltraud M Kriven","doi":"10.1107/S2052520624001598","DOIUrl":"10.1107/S2052520624001598","url":null,"abstract":"<p><p>The NaZr₂P₃O₁₂ family of materials have shown low and tailorable thermal expansion properties. In this study, SrZr₄P₆O₂₄ (SrO·4ZrO₂·3P₂O₅), CaZr₄P₆O₂₄ (CaO·4ZrO₂·3P₂O₅), MgZr₄P₆O₂₄ (MgO·4ZrO₂·3P₂O₅), NaTi₂P₃O₁₂ [½(Na₂O·4TiO₂·3P₂O₅)], NaZr₂P₃O₁₂ [½(Na₂O·4ZrO₂·3P₂O₅)], and related solid solutions were synthesized using the organic-inorganic steric entrapment method. The samples were characterized by in-situ high-temperature X-ray diffraction from 25 to 1500°C at the Advanced Photon Source and National Synchrotron Light Source II. The average linear thermal expansion of SrZr₄P₆O₂₄ and CaZr₄P₆O₂₄ was between -1 × 10^-6 per °C and 6 × 10^-6 per °C from 25 to 1500°C. The crystal structures of the high-temperature polymorphs of CaZr₄P₆O₂₄ and SrZr₄P₆O₂₄ with R3c symmetry were solved by Fourier difference mapping and Rietveld refinement. This polymorph is present above ∼1250°C. This work measured thermal expansion coefficients to 1500°C for all samples and investigated the differences in thermal expansion mechanisms between polymorphs and between compositions.</p>","PeriodicalId":7320,"journal":{"name":"Acta crystallographica Section B, Structural science, crystal engineering and materials","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10994170/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140183514","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}