Journal of Chemical Crystallography最新文献

{"title":"Synthesis, Crystal Structure and Spectral Characterization of a New Caesium–Sodium-Isopolyvanadate: Photodegradation of Methylene Blue Dye","authors":"Tahmineh Kohanfekr,&nbsp;Mohammad Hakimi,&nbsp;Hasan Ali Hosseini,&nbsp;Michal Dusek,&nbsp;Monika Kucerakova","doi":"10.1007/s10870-024-01005-6","DOIUrl":"10.1007/s10870-024-01005-6","url":null,"abstract":"<div><p>A new aqua-tricaesium-sodium polymetavanadate compound, [Cs₃Na(VO₃)₄(H₂O)] (<b>1</b>), was synthesized by reacting caesium chloride and sodium metavanadate at ambient pH. The structure was characterized and identified using single-crystal X-ray diffraction, Fourier-transform infrared spectroscopy, Raman spectroscopy, and energy dispersive X-ray analysis (EDS). Compound (<b>1</b>) crystallizes in an orthorhombic system with a Pnma space group, and cell parameters a = 11.6554(4), b = 8.3408(2), c = 16.1121(5). Vanadium has tetrahedral coordination connected to the next vanadium atom through an oxygen bridge. The infinite zigzag metavanadate chains formed by corner-sharing VO₄ tetrahedral constitute a1D building block. The chains were laterally connected through Cs, Na, and H₂O. This connectivity generates continuous 2D layers within the ab plane. The photocatalytic performance of (<b>1</b>) was evaluated by measuring the degradation of methylene blue under visible light. The results confirmed the efficiency of the photocatalytic activity because of the narrowed bandgap energy of 2.18 eV, and 85% degradation rate, making it suitable for absorbing visible light.</p><h3>Graphical Abstract</h3><p>The paper reports the synthesise and characterization of a new isopolyvanadate compound, [Cs₃Na(VO₃)₄H₂O], which contains vanadim in the five oxidation state with tetrahedral coordination.  It forms metavanadate chains interconnected by caesium and sodium cations. The photocatalytic activity was tested by degrading methylen blue under visible light irradiation. The results showed decent activity attributed to the narrowed bandgap energy of 2.18 eV.</p>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 2","pages":"132 - 139"},"PeriodicalIF":0.4,"publicationDate":"2024-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140033157","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"The Pseudo Symmetric Crystal Structure of 1,4-Diazabicyclo[2·2·2]octane-1,4-diium bis(5-hydroxy-2,4-dinitrophenolate)","authors":"Rüdiger W. Seidel,&nbsp;Richard Goddard,&nbsp;Tsonko M. Kolev","doi":"10.1007/s10870-023-01004-z","DOIUrl":"10.1007/s10870-023-01004-z","url":null,"abstract":"<div><p>Reaction of 4,6-dinitroresorcinol (<b>1</b>) and the nitrogen base 1,4-diazabicyclo[2·2·2]octane (<b>2</b>) affords the 1:2 salt and proton-transfer compound 1,4-diazabicyclo[2·2·2]octane-1,4-diium bis(5-hydroxy-2,4-dinitrophenolate) (<b>3</b>). Compound <b>3</b> crystallizes in the triclinic crystal system (space group <i>P</i>-1) with <i>a</i> = 8.3242(5) Å, <i>b</i> = 11.9915(7) Å, <i>c</i> = 12.4595(7) Å, <i>α</i> = 116.282(2)°, <i>β</i> = 100.576(3)°, <i>γ</i> = 101.051(2)°, 1042.30(11) ų and <i>Z</i> = 2. The dication <b>2</b>-<span>({text{H}}_{2}^{2+})</span> forms charge assisted donating bifurcated N⁺−H⋅⋅⋅O⁻ hydrogen bonds to the phenolate moieties of two monoanions of <b>1</b>. The latter exhibit an intramolecular O−H⋅⋅⋅O hydrogen bond between the hydroxy group and the nitro group in <i>ortho</i> position. The crystal structure of <b>3</b> features <i>pseudo B</i>-centering of the lattice, which relates the two crystallographically distinct monoanions of <b>1</b> by a <i>pseudo</i> translation. The possible <i>B</i>-centring is broken by the ethylene groups of <b>2</b>-H₂²⁺, which are related in neighbouring molecules by centres of symmetry.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div><div><p>The 1:2 proton-transfer compound 1,4-diazabicyclo[2.2.2]octane-1,4-diium bis(5-hydroxy-2,4-dinitrophenolate) features pseudo <i>B</i>-centering of the lattice.</p></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 2","pages":"125 - 131"},"PeriodicalIF":0.4,"publicationDate":"2024-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-023-01004-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139764650","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal Structure of Tetrachloroferrate(III) Complex with Methylene Blue","authors":"Vahobjon Kh. Sabirov","doi":"10.1007/s10870-023-01003-0","DOIUrl":"10.1007/s10870-023-01003-0","url":null,"abstract":"<div><p>The crystal structure of tetrachloroferrate(III) complex with methylene blue, [Mb]⁺[FeCl₄]⁻ (where [Mb]⁺ methylthioninium or 3,7-bis(dimethylamino)-phenothiazine-5-ium cation), has been prepared by mechanochemical way and studied by the single crystal X-ray crystallography. The crystal structure of title compound is built from by [FeCl₄]⁻ tetrahedral ion and planar [Mb]⁺ counter ions. The [Mb]⁺ cation is linked in the 3D network by the C–H···Cl hydrogen bonds and is stacked in an antiparallel fashion with the sulfur atom disposed alternatively on an opposite sides of the stacking. The interplanar distance between two neighboring aromatic cycles is 3.431 Å, and a centroids–centroids distance between thiazine rings is 3.975 Å. Dihedral angle between aromatic rings is 1.6°. Intermolecular short contacts were analyzed by 3D Hirshfeld surfaces method and 2D fingerprint plots. Intermolecular interaction energy between two neighboring Mb⁺ cation pair was calculated by using of CE-B3LYP/6-31G(d,p) theoretical level.</p><h3>Graphical Abstract</h3><p>The π···π stacking interactions were found plays an important role in the crystal structure formation of the FeCl₃ complex with methylene blue, and calculation by the CrystalExlorer17.5 program indicates that π···π interaction energy between two neighboring methylene blue cations is −33.5 kJ/mol.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"114 - 123"},"PeriodicalIF":0.4,"publicationDate":"2024-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139587549","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Metal Complexes of a Thiosemicarbazone with Heterocyclic Bases as Coligands: Spectral Characterization, Crystal Structures, DFT and In silico Docking Studies","authors":"Nimya Ann Mathews,&nbsp;M. Sithambaresan,&nbsp;Savaş Kaya,&nbsp;Samir Chtita,&nbsp;M. R. Prathapachandra Kurup","doi":"10.1007/s10870-023-01001-2","DOIUrl":"10.1007/s10870-023-01001-2","url":null,"abstract":"<div><p>Copper(II) and zinc(II) complexes, [Cu(esct)(4-pico)] (<b>1</b>), [Zn(esct)(5,5′-dmbipy)]·H₂O (<b>2</b>), [Cu(esct)(5,5′-dmbipy)] (<b>3</b>), (where H₂esct = 3-ethoxysalicylaldehye-N⁴-cyclohexylthiosemicarbazone) were synthesized by reacting copper acetate/zinc acetate with the thiosemicarbazone derivative (H₂esct) along with heterocyclic bases. The thiosemicarbazone forms doubly deprotonated anions in all the complexes to coordinate via thiolate S, azomethine N and phenolate O atoms. The complexes were characterized by various spectroscopic techniques like infrared, UV–vis, ¹H NMR and EPR spectra. The single crystal XRD studies confirmed the structures. All the three complexes got crystallized in triclinic space group <i>P</i> <span>(overline{1 }.)</span> Complexes are found to have four, five and six coordination around the metal center. The importance of van der Waals interactions in them is explained by Hirshfeld surface analysis. We have used Density Functional Theory (DFT) methods and optimized ground states of the studied complexes using the Gaussian 09 package. Electrostatic potential plots of complexes were investigated. Further, docking studies were carried out with various Epidermal Growth Factor Receptor (EGFR) enzymes.</p><h3>Graphical Abstract</h3><p>Three mixed ligand Cu(II) and Zn(II) complexes prepared from a thiosemicarbazone showed interesting geometries and structures</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"99 - 113"},"PeriodicalIF":0.4,"publicationDate":"2023-12-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139070205","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"The Crystal Structure of a Catena-Triglycinium-µ-Chlorido-Tetrachloridocuprate(II) Glycine Co-crystal","authors":"M. O. Mazurin,&nbsp;D. S. Tsvetkov,&nbsp;P. A. Slepukhin","doi":"10.1007/s10870-023-01002-1","DOIUrl":"10.1007/s10870-023-01002-1","url":null,"abstract":"<div><p>A new complex compound, catena-triglycinium-µ-chlorido-tetrachloridocuprate(II) glycine co-crystal (or glycine-triglycinium pentachlorocuprate), {(C₂H₆NO₂)₃CuCl₅·(C₂H₅NO₂)}_n, was synthesized and studied by single crystal X-ray diffraction (SC XRD) and mid-range infrared spectroscopy. The compound crystallizes in a non-centrosymmetric triclinic <i>P</i>1 space group with lattice parameters <i>a</i> = 5.1277(2) Å, <i>b</i> = 9.1412(6) Å, <i>c</i> = 12.2023(5) Å, <i>α</i> = 101.407(4)°, <i>β</i> = 97.460(3)°, <i>γ</i> = 105.832(4)°, Z = 1. The unit cell contains four glycine ions—three glycinium cations and single zwitter-ion—linked through hydrogen bonds network. The anionic part of the compound is presented by infinite chains [CuCl₆]_n of distorted (elongated) octahedra, connected by vertices and alternating direction of elongated axis. Positions of hydrogen atoms were refined using geometry optimization via density functional theory (DFT) approach. Thermogravimetric analysis (TGA) showed the title compound to be stable in air atmosphere up to ∼ 388‒393 K and decomposes upon further heating.</p><h3>Graphical Abstract</h3><p>Unit cell content of the glycine-triglycinium pentachlorocuprate, determined by the SC XRD analysis</p>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"84 - 98"},"PeriodicalIF":0.4,"publicationDate":"2023-12-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138945522","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Warfarin Tautomers in Solution: A Structural, Computational and Thermodynamic Study","authors":"Daniel A. Osborne,&nbsp;Edward Danielyan,&nbsp;Khoi Hoang,&nbsp;Edward J. Valente","doi":"10.1007/s10870-023-00999-9","DOIUrl":"10.1007/s10870-023-00999-9","url":null,"abstract":"&lt;div&gt;&lt;p&gt;Variable temperature NMR spectroscopic measurements on (S)-warfarin [open-form: 3-(1′-phenyl-3′-oxobut-1′-yl)-4-hydroxycoumarin] in CDCl&lt;sub&gt;3&lt;/sub&gt;, CD&lt;sub&gt;3&lt;/sub&gt;OD and d&lt;sub&gt;6&lt;/sub&gt;-DMSO generally showed tautomeric compositions in the order &lt;i&gt;trans&lt;/i&gt; (2S,4S) coumarin hemiketal &gt; &lt;i&gt;cis&lt;/i&gt; (2R,4S) coumarin hemiketal &gt; open (S) coumarin enol in slow dynamic equilibrium over temperature ranges rising modestly from ambient. A computational (DFT-M06-2X) examination of the lower energy tautomers including coumarin and chromone open and cyclic forms (gas phase, chloroform or DMSO fields) was consistent with the general solution compositions. The crystal and molecular structures for model compounds of the major solution tautomers are reported: (2S,4S)-warfarin methyl ketal [orthorhombic, &lt;i&gt;P&lt;/i&gt;2&lt;sub&gt;1&lt;/sub&gt;2&lt;sub&gt;1&lt;/sub&gt;2&lt;sub&gt;1&lt;/sub&gt;], (2R,4S)-warfarin methyl ketal [orthorhombic, &lt;i&gt;P&lt;/i&gt;2&lt;sub&gt;1&lt;/sub&gt;2&lt;sub&gt;1&lt;/sub&gt;2&lt;sub&gt;1&lt;/sub&gt;], (&lt;i&gt;rac&lt;/i&gt;)-warfarin-4-methyl ether [monoclinic, &lt;i&gt;P&lt;/i&gt;2&lt;sub&gt;1&lt;/sub&gt;/&lt;i&gt;n&lt;/i&gt;], and the open chromone (S)-warfarin-2-methyl ether [monoclinic, &lt;i&gt;P&lt;/i&gt;2&lt;sub&gt;1&lt;/sub&gt;, Z = 8]. A combination of direct integration and line-fitting methods were used to determine solution (S)-warfarin tautomer compositions. As temperatures were increased, the concentrations of the open coumarin form increased at the expense of the cyclic hemiketals. Equilibrium constants were used to determine the standard free-energy differences for the two open-cyclic equilibria (&lt;i&gt;trans&lt;/i&gt; hemiketal &lt;span&gt;(rightleftharpoons)&lt;/span&gt; open, open &lt;span&gt;(rightleftharpoons)&lt;/span&gt; &lt;i&gt;cis&lt;/i&gt; hemiketal, respectively) in three solvents: CDCl&lt;sub&gt;3&lt;/sub&gt; [+ 3.7(4), − 2.8(6) kJ/mol], CD&lt;sub&gt;3&lt;/sub&gt;OD [+ 7.6(16), − 4.7(9) k/mol], d&lt;sub&gt;6&lt;/sub&gt;-DMSO [+ 3.5(7), − 1.1(2) kJ/mol]. Standard enthalpy and entropy differences were also determined from van’t Hoff analysis. Rates of the respective reactions were estimated from line-widths for the cyclic hemiketals and solution equilibrium compositions for each species. Eyring analysis gave ΔG&lt;sup&gt;‡&lt;/sup&gt;, ΔH&lt;sup&gt;‡&lt;/sup&gt;, and ΔS&lt;sup&gt;‡&lt;/sup&gt;, respectively, for the forward and reverse reactions of coumarin &lt;i&gt;trans&lt;/i&gt; hemiketal &lt;span&gt;(rightleftharpoons)&lt;/span&gt; open-form and for the open-form &lt;span&gt;(rightleftharpoons)&lt;/span&gt; &lt;i&gt;cis&lt;/i&gt; hemiketal. Negative entropic contributions to the observed transition state energies were consistent with solvent or solute ordering in the prototropic reactions. Open-form NMR signals were broader than could be accounted for by the open-cyclic equilibria alone, increasingly so in polar and protic solvents and with rising temperatures. While a conformational equilibrium may operate, an increasingly faster intermediate dynamic equilibrium between open coumarin-chromone tautomers may be a more likely explanation.&lt;/p&gt;&lt;h3&gt;Graphical Abstract&lt;/h3&gt;&lt;p&gt;Structures of methylated warfarin tautomers and computational models enabled assignment of overlapping warfarin tautomeric NMR spectra and t","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"64 - 83"},"PeriodicalIF":0.4,"publicationDate":"2023-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138687271","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"New Tetraruthenium Cluster from the Thermolysis of [Ru3(CO)10(μ-dppm)]: Crystal Structure of [HRu4(CO)9(μ3-PhPCH2PPh2) (μ3,η2:η1:η1-C6H4)]","authors":"Md. Abdullah Al Mamun,&nbsp;Tazul Islam,&nbsp;Subas Rajbangshi,&nbsp;Shishir Ghosh,&nbsp;Michael G. Richmond,&nbsp;Shariff E. Kabir","doi":"10.1007/s10870-023-00998-w","DOIUrl":"10.1007/s10870-023-00998-w","url":null,"abstract":"<div><p>Thermolysis of [Ru₃(CO)₁₀(μ-dppm)] (<b>1</b>) in refluxing benzene, followed by chromatographic separation by TLC, afforded the new cluster [HRu₄(CO)₉(μ₃-PhPCH₂PPh₂)(μ₃,η²:η¹:η¹-C₆H₄)] (<b>10</b>) in 7% yield in addition to the previously reported clusters [Ru₃(CO)₉{µ₃-PhPCH₂PPh(C₆H₄)}] (<b>2</b>) and [HRu₄(CO)₉(μ₄-PhPCH₂PPh₂)(μ₄,η⁶:η¹:η¹-C₆H₄)] (<b>8</b>) in 70% and 4% yields, respectively. The molecular structure of <b>10</b> has been determined by single-crystal X-ray diffraction analysis. Compound <b>10</b> possesses a Ru₄ metal core where two of the six triangular faces are capped by μ₃,η²:η¹:η¹-C₆H₄ (benzyne) and µ₃-PhPCH₂PPh₂ ligands. Compound <b>10</b> transforms to the known cluster [HRu₄(CO)₉(μ₃-PhPCH₂PPh₂)(μ₄,η⁶:η¹:η¹-C₆H₄)] (<b>8</b>) slowly at 80 °C. The bonding in the new cluster <b>10</b> has been investigated by electronic structure calculations.</p><h3>Graphical Abstract</h3><p>A new tetraruthenium cluster has been isolated and structurally characterized from the thermolysis of [Ru₃(CO)₁₀(μ-dppm)] at 80 °C.</p>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"54 - 63"},"PeriodicalIF":0.4,"publicationDate":"2023-12-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138523664","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal and Molecular Structures of Three Co-crystals from 1,3-Dimethyl-3,7-dihydro-1H-purine-2,6-dione and Carboxylic Acids","authors":"Zhaozhi Li,&nbsp;Xianhong Wen,&nbsp;Shouwen Jin,&nbsp;Xingjun Gao,&nbsp;Weiqiang Xu,&nbsp;Yaoqi Zhen,&nbsp;Chenzhe Shi,&nbsp;Daqi Wang","doi":"10.1007/s10870-023-01000-3","DOIUrl":"10.1007/s10870-023-01000-3","url":null,"abstract":"<div><p>The preparation, X-ray crystal structure, Fourier Transform infrared (FTIR) spectroscopy, and elemental analysis of the three complexes (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (2,6-dichlorobenzoic acid)₂: H₂O [(tp)· (Hbza)₂ · H₂O, Hdcba = 2,6-dichlorobenzoic acid] (<b>1</b>) (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (2-pyrazinecarboxylic acid) [(tp) · (Hpyca), Hpyca = 2-pyrazinecarboxylic acid] (<b>2</b>) and (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (3-nitrophthalic acid) [(tp) · (Hntpa)] (<b>3</b>) based on 1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione, 2,6-dichlorobenzoic acid 2-pyrazinecarboxylic acid, and 3-nitrophthalic acid are reported. XRD and FTIR analysis indicated that they are all co-crystal. <b>1</b> crystallizes in the monoclinic, space group <i>P</i>2₁/<i>n</i>, with a = 7.1019(7) Å, b = 12.9494(12) Å, c = 26.253(3) Å, β = 93.536(3)°, V = 2409.8(4) ų, Z = 4. <b>2</b> crystallizes in the monoclinic, space group <i>P</i>2₁/<i>c</i>, with a = 6.9863(7) Å, b = 25.437(3) Å, c = 7.3987(7) Å, β = 95.152(2)°, V = 1309.5(2) ų, Z = 4. <b>3</b> crystallizes in the monoclinic, space group <i>P</i>2₁/<i>n</i>, with a = 14.2133(15) Å, b = 8.2333(9) Å, c = 15.3860(17) Å, <i>β</i> = 117.236(5)º, V = 1600.9(3) ų, Z = 4. The imidazole-carboxylic acid synthon of the CO₂H···N type is observed in all the co-crystal. The imidazole H–N also donated the N–H···O hydrogen bonds in all cases. Apart from the classical hydrogen bonds, the auxiliary expanding interactions as CH···O, CH₃···O, CH···Cl, O···O, Cl···O, Cl···Cl, Cl···π, O···π, and π···π also play important roles in the structure extension. For the coexistence of the various weak interactions these structures adopted the most common R₂²(7) supramolecular synthon. In conclusion, we have shown that 2D–3D connections can be constructed by the collective non-covalent interactions.</p><h3>Graphical Abstract</h3><p>\u0000In the three prepared supramolecular assemblies there are plenty of weak nonbonding interactions such as directional hydrogen bonds of O–H···N, N-H···O, O–H···O, intra- and interchain CH···O, CH₃···O, CH···Cl, O···O, Cl···O, Cl···Cl, Cl···π, O···π, and π···π interactions, on account of these collective weak interactions, these compounds displayed the 2D–3D framework structures.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"41 - 53"},"PeriodicalIF":0.4,"publicationDate":"2023-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138523681","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal Structure of 2-((E)-((Z)-3-(((4-hydroxyphenyl)amino)methylene)-4-oxocyclohexa-1,5-dien-1-yl)diazenyl)benzoic Acid and Synthesis, Spectroscopy, and DFT Study of Its Dibutyltin(IV) Complex","authors":"Pratima Debnath,&nbsp;Chinmoy Majumder,&nbsp;Arnab Bhattacharya,&nbsp;Paresh Debnath,&nbsp;Subhadip Roy,&nbsp;Alexander S. Novikov,&nbsp;Manojit Roy,&nbsp;Tarun Kumar Misra","doi":"10.1007/s10870-023-00996-y","DOIUrl":"10.1007/s10870-023-00996-y","url":null,"abstract":"<div><p>The structure of the 2-((<i>E</i>)-((<i>Z</i>)-3-(((4-hydroxyphenyl)amino)methylene)-4-oxocyclohexa-1,5-dien-1-yl)diazenyl)benzoic acid (H₃L) was confirmed by single crystal X-ray diffraction and Hirshfeld surface analysis was used further to quantify the intermolecular interactions. It crystallized in monoclinic space group <i>P</i>2₁/c. The observed bond distances evidence that the structure exists predominately in azo-enamine tautomeric form in the solid state. A novel dibutyltin(IV) complex, [(Bu₂SnHL)₂] (<b>1</b>) was synthesized from H₃L. The complex was then characterized by studying different techniques including elemental analysis, FT-IR, and NMR (¹H, ¹³C, and ¹¹⁹Sn) spectroscopy. In solution state, the molar mass of the compound was confirmed by Mass spectrometry. Spectroscopy study guides to predict the structure of the complex which is supposed to be a cyclic dimer [(Bu₂SnHL)₂] and Sn(IV) adopts a six-coordinated geometry. However, in solution Sn(IV) adopts four coordinated distorted tetrahedral geometry which was supported by ¹¹⁹Sn NMR spectroscopy (δ_Sn(119), 126.34 ppm) and EI-MS results of the complex ion ([C₂₈H₃₂N₃O₄Sn]⁺,m/z 593.1). Further, the structures in solid and solution state were supported by developing their optimized structures and IR data from the DFT calculation.</p><h3>Graphical Abstract</h3><p>The crystal structure of the ligand is in azo-enamine tautomeric form and in accordance with DFT study, its dibutyltin(IV) complex is a cyclic dimer, (Bu₂SnHL)₂, which becomes monomer in solution.</p>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"28 - 40"},"PeriodicalIF":0.4,"publicationDate":"2023-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138523679","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Exploring Cyclic Hydrogen Bonds and Polymorphic Potential in 1,2-Diols Through Hirshfeld Analyses and Fingerprint Plots","authors":"Mónica Farfán-Paredes,&nbsp;Ma. Eugenia Ochoa,&nbsp;Rosa Santillan,&nbsp;Norberto Farfán","doi":"10.1007/s10870-023-00997-x","DOIUrl":"10.1007/s10870-023-00997-x","url":null,"abstract":"<div><p>The molecular environment in the crystal of [1,1′-bi(cyclopentane)-1,1′-diol] <b>D-1</b> and [1,1′-bi(cyclohexane)-1,1′-diol] <b>D-2</b> were comparatively investigated using X-ray diffraction, Hirshfeld surface analysis and two-dimensional plotting of the normalized interatomic distance. Different ways of crystallization of <b>D-1</b> led to polymorphism. Studying the differences between the chemical environments of polymorphic molecules is the key for understanding the structure in the solid state. Hirshfeld analyses along with fingerprint plots revealed the differences between the two polymorphs of <b>D-1</b> with <i>anti-</i> and <i>syn-</i>conformation, and the similarities between <b>D-1</b> and <b>D-2</b> that show the same six hydrogen bonds motif. A co-crystal <b>DB</b> between <b>D-2</b> and a hexahydroisobenzofuran derivative was also analyzed. Fingerprint plots show a distinctive pair of spikes in the structures with cyclic hydrogen bonds as well as information about the contribution of O–H⋯O/O⋯H–O interactions, that is different for each system despite having the same number of –OH groups. Knowledge of the conformation and the intermolecular interactions is crucial to understand its role in this kind of systems and for their potential use in pharmaceutical industry, supramolecular engineering, catalysis, and design of new materials.</p><h3>Graphical Abstract</h3><p>Hirshfeld analyses along with fingerprint plots revealed the differences between two polymorphs with <i>anti-</i> and <i>syn-</i>conformation, and the similarities between compounds that show the same six hydrogen bonds motif.</p>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"18 - 27"},"PeriodicalIF":0.4,"publicationDate":"2023-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134901245","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}