Journal of Chemical Crystallography最新文献

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Synthesis, Crystal Structure, FT-IR and UV-Vis Spectra of Tetranuclear Copper (II) Complex with 4-methoxypyridine as Co-Ligand 以4-甲氧基吡啶为配体的四核铜配合物的合成、晶体结构、红外光谱和紫外可见光谱
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-08-21 DOI: 10.1007/s10870-025-01059-0
Ugur Erkarslan, Gorkem Oylumluoglu, Ozay Eroglu, Hanife Sevval Dere, Elif Gungor, Hulya Kara Subasat, Adem Donmez
{"title":"Synthesis, Crystal Structure, FT-IR and UV-Vis Spectra of Tetranuclear Copper (II) Complex with 4-methoxypyridine as Co-Ligand","authors":"Ugur Erkarslan,&nbsp;Gorkem Oylumluoglu,&nbsp;Ozay Eroglu,&nbsp;Hanife Sevval Dere,&nbsp;Elif Gungor,&nbsp;Hulya Kara Subasat,&nbsp;Adem Donmez","doi":"10.1007/s10870-025-01059-0","DOIUrl":"10.1007/s10870-025-01059-0","url":null,"abstract":"<div><p>A methanol solvate of the tetranuclear Cu(II) complex with 4-methoxypyridine (4-MOP) as co-ligand have been synthesized, [Cu<sub>4</sub>OCl<sub>6</sub>.(4-MOP)<sub>4</sub>].CH<sub>2</sub>OH, (4-MOP = 4-methoxypyridine) and characterized by IR, UV–Vis spectroscopy and single crystal X-ray diffraction. The complex exhibits a tetrahedral {Cu<sub>4</sub>O} core, where four Cu(II) ions are bridged by six chloride ligands and further stabilized through coordination with 4-methoxypyridine ligands. Each copper center displays a distorted trigonal bipyramidal geometry. Intermolecular C–H···Cl and C–H···O hydrogen bonds interconnect the molecules, forming a three-dimensional supramolecular framework. Spectroscopic data, including UV-Vis and FT-IR, substantiate the formation of the Cu<sub>4</sub>O cluster and align with the structural observations. These findings offer valuable insights into the coordination behavior and supramolecular organization of µ<sub>4</sub>-oxo copper complexes, presenting a useful model for biomimetic systems and a potential foundation for applications in catalysis and material science.</p><h3>Graphical Abstract</h3><p>A rare example of a µ<sub>4</sub>-oxo-bridged tetranuclear Cu(II) complex stabilized by 4-methoxypyridine ligands has been selectively synthesized and structurally characterized. This is among the few known Cu₄OCl₆ type architectures incorporating 4-MOP, revealing a well-defined {Cu<sub>4</sub>O} core and a 3D supramolecular network through weak hydrogen bonding.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 4","pages":"281 - 289"},"PeriodicalIF":0.6,"publicationDate":"2025-08-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145204639","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}
引用次数: 0
A Dinuclear Pd Complex with the bis(Pyridyltriazole) Ligand m-xpt: [Pd2(m-xpt)2](DMSO)6(BF4)4 具有双(吡啶基三唑)配体的双核Pd配合物m-xpt: [Pd2(m-xpt)2](DMSO)6(BF4)4
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-08-18 DOI: 10.1007/s10870-025-01058-1
Sen Gao, Frank R. Fronczek, Andrew W. Maverick
{"title":"A Dinuclear Pd Complex with the bis(Pyridyltriazole) Ligand m-xpt: [Pd2(m-xpt)2](DMSO)6(BF4)4","authors":"Sen Gao,&nbsp;Frank R. Fronczek,&nbsp;Andrew W. Maverick","doi":"10.1007/s10870-025-01058-1","DOIUrl":"10.1007/s10870-025-01058-1","url":null,"abstract":"<div><p>The title compound (<b>1</b>) was synthesized through reaction between Pd(CH<sub>3</sub>CN)<sub>4</sub>(BF<sub>4</sub>)<sub>2</sub> and <i>m</i>-xylylenebis(pyridyltriazole) (<i>m</i>-xpt) in a mixture of CH<sub>2</sub>Cl<sub>2</sub> and CH<sub>3</sub>CN. The solid product was crystallized by vapor diffusion of ethyl ether into a DMSO solution. In the crystal structure of <b>1</b>, square-planar <i>trans</i>-[Pd(pyridyltriazole)<sub>2</sub>]<sup>2+</sup> groups are joined by <i>m</i>-xylylene bridges to make centrosymmetric [Pd<sub>2</sub>(<i>m</i>-xpt)<sub>2</sub>]<sup>4+</sup> cations with Pd⋯Pd = 5.1337(4) Å. As in previously published structures with the isomeric <i>o</i>-xpt ligand, ([Ag<sub>2</sub>(<i>o</i>-xpt)<sub>2</sub>]<sup>2+</sup> and [Pd<sub>2</sub>(<i>o</i>-xpt)<sub>2</sub>]<sup>4+</sup>), the Pd(pyridyltriazole)<sub>2</sub> planes in <b>1</b> make close π contact (3.302 Å); this is accomplished by twisting of the <i>m</i>-xpt bridging groups, so that the longer Pd⋯Pd vector makes a 40° angle with the Pd(pyridyltriazole)<sub>2</sub> planes.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div><p>The crystal structure of the title compound shows a Pd⋯Pd distance approximately as expected (5.1337(4) Å), but with its <i>m</i>-xylylene groups twisted in order to permit close π–π interactions (3.302 Å) between its Pd(pyridyltriazole)<sub>2</sub> planes.</p></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 4","pages":"275 - 280"},"PeriodicalIF":0.6,"publicationDate":"2025-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-025-01058-1.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145204630","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}
引用次数: 0
Crystal Growth and Characterization of a New Tetrameric Complex of Ba(II) with Pamoic Acid 一种新的Ba(II) - Pamoic酸四聚物的晶体生长和表征
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-08-13 DOI: 10.1007/s10870-025-01057-2
S. Shibu Prasad
{"title":"Crystal Growth and Characterization of a New Tetrameric Complex of Ba(II) with Pamoic Acid","authors":"S. Shibu Prasad","doi":"10.1007/s10870-025-01057-2","DOIUrl":"10.1007/s10870-025-01057-2","url":null,"abstract":"<div><p>A new tetrameric complex of Ba(II), [Ba<sub>4</sub>(PA)<sub>4</sub>(H<sub>2</sub>O)<sub>20</sub>]·4H<sub>2</sub>O (PA = pamoate) has been prepared by gel diffusion technique at ambient condition. The grown crystals were characterized by elemental analysis, single crystal X-ray diffraction studies, thermogravimetry, FT-IR and UV–visible spectral studies. The single crystal X-ray diffraction studies show that the crystal structure consists of two different types of nine coordinated Ba centers (Ba1 and Ba2). In addition to the carboxylate groups of pamoate, two coordinated water also interconnect the Ba(II) centers. The carboxylate groups of pamoate exhibit monodentate, bismonodentate and bidentate, coordination modes with Ba(II) ions. Hydrogen bonding further stabilizes the crystal structure. Photoluminescence studies were also carried out.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div><p>A new tetrameric complex of Ba(II) with pamoic acid (H<sub>2</sub>PA) of formula [Ba<sub>4</sub>(PA)<sub>4</sub>(H<sub>2</sub>O)<sub>20</sub>]·4H<sub>2</sub>O (BaPA) has been prepared by gel diffusion technique at ambient condition and is characterized by various analytical techniques.</p></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 4","pages":"267 - 274"},"PeriodicalIF":0.6,"publicationDate":"2025-08-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145204634","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}
引用次数: 0
Hydrothermal Synthesis and Structural Characterization of a New Lead Tri-magnesium Phosphate PbMg3(HPO4)(PO4)2 新型磷酸铅三镁PbMg3(HPO4)(PO4)2的水热合成及结构表征
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-08-13 DOI: 10.1007/s10870-025-01056-3
Ahmed Ould Saleck, Cyrille Albert-Mercier, Claudine Follet-Houttemane, Abderrazzak Assani, Mohamed Saadi, Lahcen El Ammari
{"title":"Hydrothermal Synthesis and Structural Characterization of a New Lead Tri-magnesium Phosphate PbMg3(HPO4)(PO4)2","authors":"Ahmed Ould Saleck,&nbsp;Cyrille Albert-Mercier,&nbsp;Claudine Follet-Houttemane,&nbsp;Abderrazzak Assani,&nbsp;Mohamed Saadi,&nbsp;Lahcen El Ammari","doi":"10.1007/s10870-025-01056-3","DOIUrl":"10.1007/s10870-025-01056-3","url":null,"abstract":"<div><p>A new lead tri-magnesium phosphate PbMg<sub>3</sub>(HPO<sub>4</sub>)(PO<sub>4</sub>)<sub>2</sub> was synthesized by hydrothermal method and characterized by single crystal X-ray diffraction. This phosphate crystallizes in the monoclinic system with space group <i>I</i>2<i>/m</i> and unit cell parameters <i>a</i> = 6.6403(2)Å, <i>b</i> = 13.1169(5) Å, <i>c</i> = 10.7153(4) Å and β = 90.194 (1)°. The structure consists of two edge-sharing [MgO<sub>6</sub>] octahedra linked to [PO<sub>4</sub>] or [HPO<sub>4</sub>] tetrahedra to build [Mg<sub>2</sub>P<sub>2</sub>O<sub>14</sub>] and [Mg<sub>2</sub>H<sub>2</sub>P<sub>2</sub>O<sub>14</sub>] moieties, which are interconnected together through vertices to form a sheet parallel to (1 0 0) plan. In addition, an infinite chain ([MgPO<sub>9</sub>]<sub>∞</sub>) formed by the sharing of a vertex between the [MgO<sub>6</sub>] octahedron and the [PO<sub>4</sub>] tetrahedron ensures the connection of the sheets to form a three-dimensional structure containing tunnels parallel to the <i>b</i> and <i>c</i> axes. The Pb<sup>2+</sup> and H<sup>+</sup> cations are located in disordered sites in these tunnels. The structure of this phosphate exhibits also a strong hydrogen bond.</p><h3>Graphical Abstract</h3><p>(A) and (C) Polyhedral representation of the structure showing the tunnels along the [010] and [001] directions that house Pb and H atoms. The dashed lines in the tunnels of (C) represent the hydrogen bond O1–H1…O1<sup>i</sup>. (B) Infinite chain [MgPO<sub>9</sub>]<sub>∞</sub> formed by alternating [MgO<sub>6</sub>] octahedra and [PO<sub>4</sub>] tetrahedra, which connect the layers stacked along the <i>c</i>-axis.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 4","pages":"259 - 266"},"PeriodicalIF":0.6,"publicationDate":"2025-08-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145204638","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}
引用次数: 0
Supramolecular Assembly and Structural Insights of 2,4,6-triaminopyrimidinium bis(3,5-dinitrosalicylato) Diaquamagnesate(II) Dihydrate 2,4,6-三氨基嘧啶双(3,5-二硝基水杨酸酯)双水镁酸酯(II)的超分子组装及结构研究
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-06-19 DOI: 10.1007/s10870-025-01055-4
Marimuthu Sangavi, Marimuthu Mohana, Ray J. Butcher
{"title":"Supramolecular Assembly and Structural Insights of 2,4,6-triaminopyrimidinium bis(3,5-dinitrosalicylato) Diaquamagnesate(II) Dihydrate","authors":"Marimuthu Sangavi,&nbsp;Marimuthu Mohana,&nbsp;Ray J. Butcher","doi":"10.1007/s10870-025-01055-4","DOIUrl":"10.1007/s10870-025-01055-4","url":null,"abstract":"<div><p>The monomeric magnesium complex, C₄H₈N₅⁺[Mg(C₇H<sub>2</sub>N₂O₇)₂(H₂O)₂]·2 H₂O, crystallizes in a triclinic P-1 space group. In this structure, Mg(II) ion adopts an octahedral geometry. The coordination sphere around the metal center is formed by four oxygen atoms from two bidentate 3,5-dinitrosalicylate anions (DNS) in the equatorial plane, while two oxygen atoms from coordinated water molecules occupy the axial positions. Extensive hydrogen bonding stabilizes the crystal structure with the non-coordinated 2,4,6-triaminopyrimidinium cation (TAP) generating primary ring motifs such as R₂²(8) and R₂³(8), which extend into a complex three-dimensional hydrogen-bonded network. Coordinated and non-coordinated water molecules play a crucial role in maintaining the supramolecular framework by engaging in N–H…O, O–H…O and O–H…N hydrogen bonding interactions. Additionally, π–π stacking interactions contribute to the stabilization of the structure. These cooperative non-covalent interactions not only strengthen the crystal packing but also contribute to the overall stability of the supramolecular architecture, making this complex a potential candidate for future studies in crystal engineering and molecular assembly.</p></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 4","pages":"251 - 258"},"PeriodicalIF":0.6,"publicationDate":"2025-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145204637","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}
引用次数: 0
Crystal Structure and DFT Studies of Bis{(E)-2,4-di-tert-butyl-6-((2-fluorophenylimino)methyl) phenolato-N, O-}copper(II) 双{(E)-2,4-二叔丁基-6-((2-氟苯基)甲基)苯酚- n, O-}铜(II)的晶体结构和DFT研究
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-06-12 DOI: 10.1007/s10870-025-01053-6
Gökhan Alpaslan, Halil Gökce, Yelda Bingöl Alpaslan, Mustafa Macit, Namık Özdemir
{"title":"Crystal Structure and DFT Studies of Bis{(E)-2,4-di-tert-butyl-6-((2-fluorophenylimino)methyl) phenolato-N, O-}copper(II)","authors":"Gökhan Alpaslan,&nbsp;Halil Gökce,&nbsp;Yelda Bingöl Alpaslan,&nbsp;Mustafa Macit,&nbsp;Namık Özdemir","doi":"10.1007/s10870-025-01053-6","DOIUrl":"10.1007/s10870-025-01053-6","url":null,"abstract":"<div><p>A novel transition metal complex was synthesized from the reaction between the copper(II)acetate and the Schiff base ligand (<i>E</i>)-2,4-di-<i>tert</i>-butyl-6-((2-fluorophenylimino)methyl)phenol. The title complex was structurally characterized by single crystal X-ray diffraction technique. Crystallographic analysis revealed that the copper(II) center in the investigated complex is four-coordinate, consisting of two imine nitrogen atoms and two phenolic oxygen atoms from two bidentate Schiff bases. The coordination geometry is a distorted seesaw configuration with a τ4 index of 0.33. Hirshfeld surface analysis was employed to investigate the intermolecular contacts within the crystal structure using 3D <i>d</i><sub><i>norm</i></sub> surface and 2D fingerprint histograms. The fingerprint plots indicated that the dominant contacts were Van der Waals interactions (H···H, 74.3%), with C···H and H···F interactions also contributing significantly to the overall packing. Density functional theory calculations with the B3LYP/LanL2DZ level were used to calculate the molecular geometric structure of the Cu(II) complex in the ground state. The calculated values were compared with the crystallographic one. Additionally, Natural Bond Orbital (NBO) analysis was performed using the same basis set. The electronic properties of the atoms within the coordination environment and their hyperconjugative interactions were evaluated using NBO analysis.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>In this study, the synthesis of a copper(II) complex compound, some DFT calculations, single-crystal X-ray and Hirshfeld surface analyses were performed and interpreted</p></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 4","pages":"233 - 243"},"PeriodicalIF":0.6,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145204629","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}
引用次数: 0
Crystal Structure Analysis of 1, 4, 7-Trithia-10, 13-diazacyclopentadecane-9, 14-dione 1,4,7 - trithia - 10,13 -重氮环戊烷- 9,14 -二酮的晶体结构分析
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-06-12 DOI: 10.1007/s10870-025-01054-5
Timothy M.E. Jugovic, Christopher G. Hamaker
{"title":"Crystal Structure Analysis of 1, 4, 7-Trithia-10, 13-diazacyclopentadecane-9, 14-dione","authors":"Timothy M.E. Jugovic,&nbsp;Christopher G. Hamaker","doi":"10.1007/s10870-025-01054-5","DOIUrl":"10.1007/s10870-025-01054-5","url":null,"abstract":"<div>\u0000 \u0000 <p>The compound 1,4,7-trithia-10,13-diazacyclopentadecane-9,14-dione, <b>1</b>, crystallizes in the space group <i>P</i>2<sub>1</sub>/<i>c</i> with <i>a</i> = 9.3608(3) Å, <i>b</i> = 16.0333(5) Å, <i>c</i> = 9.5608(3) Å, <i>β</i> = 113.3521(14)°, and <i>Z</i> = 4. The title molecule forms chains via face-to-face N–H<sup>…</sup>O hydrogen bonds. The structure of <b>1</b> is also compared to the previously reported oxygen analog, 1,4,7-trioxa-10,13-diazacyclopentadecane-9,14-dione.</p>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 4","pages":"244 - 250"},"PeriodicalIF":0.6,"publicationDate":"2025-06-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-025-01054-5.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145204636","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}
引用次数: 0
3-(N-Alkylammonium)propanesulfonate Inner Salts, A Short Series 3-(n -烷基铵)丙磺酸盐内盐,短系列
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-05-30 DOI: 10.1007/s10870-025-01052-7
Eva R. Richman, Edward J. Valente
{"title":"3-(N-Alkylammonium)propanesulfonate Inner Salts, A Short Series","authors":"Eva R. Richman,&nbsp;Edward J. Valente","doi":"10.1007/s10870-025-01052-7","DOIUrl":"10.1007/s10870-025-01052-7","url":null,"abstract":"<div><p>Reaction of even parity primary alkyl amines with propanesultone produces 3-(<i>N</i>-alkylammonium)propanesulfonate inner salts as slightly-soluble solids in polar solvents and in good yields. A short series of amines, <i>n</i>-C<sub>n</sub>H<sub>2n+1</sub>NH<sub>2</sub> with n = 4, 6, 8, 10, was studied. Crystals of the <i>N</i>-butyl analog from water occurred as a dihydrate, orthorhombic, <i>P nma</i>, with molecules lying on mirror planes and waters in general positions. Secondary ammonium ions are hydrogen-bonded to waters of crystallization, which are hydrogen-bonded to sulfonate oxygens with only two-centered<sup>+</sup>N-H…O<sub>w</sub> and O-H…O<sup>-</sup> interactions. Beginning with the <i>N</i>-hexyl homolog, crystals are polycrystalline, fibrous and with sufficient alignment coherence to allow determination as though single crystals. The degree of fiber misalignment was 3–5<sup>o</sup>, approximately. Crystals from water are triclinic (unsolvated), <i>P</i> -1, with molecules lying between crystal (0 2 2) planes. Molecular packing shows adjacent molecules hydrogen-bonded between secondary ammonium ions and sulfonate ions in which all <sup>+</sup>N-H…(O, O’)<sup>-</sup> interactions are three-centered. Terminal alkyl groups pack in adjacent regions so that both hydrogen-bonding and dispersion attractions contribute to increasing intermolecular attractions and melting temperatures, exceeding 260 <sup>o</sup>C for the <i>N</i>-decyl homolog. The four compounds are further characterized by infrared spectroscopy and proton and carbon magnetic resonance spectroscopy and solubilities in common solvents.</p><h3>Graphical Abstract</h3><p>3-(<i>N</i>-Butylammonium)propanesulfonate zwitterions are mirror symmetric in <i>P nma</i>, while hexyl, octyl and decyl homologs are fibrous triclinic (<i>P</i> -1) structures with molecules lying approximately along the (0 1 1) planes</p><div><figure><div><div><picture><img></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 3","pages":"223 - 231"},"PeriodicalIF":0.6,"publicationDate":"2025-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144990520","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}
引用次数: 0
Crystal Structure of Methyl 2,3-di-O-benzyl-α-d-(4-2H)-Glucopyranoside 甲基2,3-二- o -苄基-α-d-(4-2H)-葡萄糖吡喃苷的晶体结构
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-05-14 DOI: 10.1007/s10870-025-01051-8
Hani Mobarak, Vadim Kessler, Lars Eriksson, Göran Widmalm
{"title":"Crystal Structure of Methyl 2,3-di-O-benzyl-α-d-(4-2H)-Glucopyranoside","authors":"Hani Mobarak,&nbsp;Vadim Kessler,&nbsp;Lars Eriksson,&nbsp;Göran Widmalm","doi":"10.1007/s10870-025-01051-8","DOIUrl":"10.1007/s10870-025-01051-8","url":null,"abstract":"<div><p>Methyl 2,3-di-<i>O</i>-benzyl-α-<span>d</span>-(4-<sup>2</sup>H)-glucopyranoside, C<sub>21</sub>H<sub>25</sub>DO<sub>6</sub>, is an intermediate used in synthesis of oligosaccharides. The hexopyranose ring has the <sup>4</sup><i>C</i><sub>1</sub> chair conformation in the crystal structure. The exocyclic groups of the hexose sugar show for the glycosidic torsion angle <i>ϕ</i> =−52.8° and for the hydroxymethyl group the <i>gauche</i>-<i>gauche</i> conformation with <i>ω</i> = −64.7°, one of the two main orientations of the latter group in hexopyranose sugars that have the <i>gluco</i>-configuration, i.e., with an equatorial hydroxyl group at C4. The benzene rings of the benzyl groups are arranged with an angle of 56.9° to each other within the molecule and show intramolecular as well as intermolecular C-H<b>···</b>π interactions. A chain of intermolecular hydrogen bonds exists along the b-axis involving O4 and O6 atoms. The experimentally observed peak in the infrared spectrum at 2159 cm<sup>− 1</sup> was ascribed to the stretching of the C4–D4 bond based on DFT calculations.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>In the structure of the monosaccharide methyl 2,3-di-<i>O</i>-benzyl-α-<span>d</span>-(4-<sup>2</sup>H)-glucopyranoside, C<sub>21</sub>H<sub>25</sub>DO<sub>6</sub>, the two hydroxyl groups HO4 and HO6 act as both donors and acceptors resulting in an intermolecular hydrogen bond chain along the b-axis direction.</p></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 3","pages":"216 - 222"},"PeriodicalIF":0.6,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-025-01051-8.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144990563","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}
引用次数: 0
Polymorph Analysis of ALZ-801 (Valiltramiprosate), a Valine-Conjugated Oral Prodrug of Tramiprosate in Late-Stage Clinical Development for Alzheimer’s Disease 缬氨酸偶联曲米普罗酸口服前药ALZ-801(缬氨酸偶联曲米普罗酸)的多态性分析
IF 0.6 4区 化学
Journal of Chemical Crystallography Pub Date : 2025-04-24 DOI: 10.1007/s10870-025-01047-4
D. Pearson, J. Amedio, J. F. Schaefer, M. Tolar, J. A. Hey
{"title":"Polymorph Analysis of ALZ-801 (Valiltramiprosate), a Valine-Conjugated Oral Prodrug of Tramiprosate in Late-Stage Clinical Development for Alzheimer’s Disease","authors":"D. Pearson,&nbsp;J. Amedio,&nbsp;J. F. Schaefer,&nbsp;M. Tolar,&nbsp;J. A. Hey","doi":"10.1007/s10870-025-01047-4","DOIUrl":"10.1007/s10870-025-01047-4","url":null,"abstract":"<div><p>ALZ-801 (valiltramiprosate) is an orally bioavailable, small-molecule inhibitor of β-amyloid (Aβ) oligomer formation in late-stage clinical development as a potential disease-modifying treatment for Alzheimer’s disease (AD). ALZ-801, (S)-3-(2-amino-3-methylbutanamido) propane-1-sulfonic acid, is a valine-conjugated prodrug of tramiprosate. Structural, polymorphic analysis of the active pharmaceutical ingredient (API) of ALZ-801 showed extra peaks when high throughput transmission mode XRPD analysis was utilized. After extensive investigation, the extra peaks were determined to be an artifact of transmission mode XRPD, which was not observed in either reflectance or capillary mode XRPD analyses. Reflectance mode XRPD was demonstrated as the most appropriate methodology to monitor the crystal form of ALZ-801 API. In conclusion, ALZ-801 API is a single, pure polymorph form.</p><h3>Graphical Abstract</h3><p>\u0000A single crystalline form of ALZ-801 is observed in a range of crystal morphologies, the risk of a change in solid form affecting the delivery of this potential new disease modifying therapy for Alzheimer’s disease is negligible</p><p>Phase light microscopy image of ALZ-801 crystal pattern 1 (single polymorph). ALZ-801 crystals occur in diverse ranges of morphologies, i.e., tetrahedron (a), bladed, needles, dodecahedron, slices(b), prismatic (c) and tabular (d) forms</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 3","pages":"206 - 215"},"PeriodicalIF":0.6,"publicationDate":"2025-04-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144990535","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}
引用次数: 0
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