Journal of Chemical Crystallography最新文献

{"title":"Polymorphism of Nicotinamide Riboside Chloride and Crystal Structure Determination of the Most Stable Crystalline Form","authors":"Dedong Wu,&nbsp;Branden Wu,&nbsp;Pingrong Wei","doi":"10.1007/s10870-023-00985-1","DOIUrl":"10.1007/s10870-023-00985-1","url":null,"abstract":"<div><p>Three crystalline forms of nicotinamide riboside chloride (NR-Cl), namely Form A, Form B and Form C, were prepared and characterized. Form A and Form B are true polymorphs of anhydrous forms, while Form C is a pseudo-polymorph of a methanolate solvate form. The relative polymorphic stability relationship among these three crystalline forms was established, and Form B was found to be the most stable form with a higher crystal density (1.591 Mg/m³) and a higher melting/decomposing temperature (123 °C) compared to that of Form A (1.512 Mg/m³ and 119 °C). The crystal structure of Form B (orthorhombic <i>P</i>2₁2₁2₁ space group, <i>a</i> = 7.0008(11) Å, <i>b</i> = 9.6465(15) Å, <i>c</i> = 17.971(3) Å, <i>V</i> = 1213.7(3) ų, <i>Z</i> = 4) was determined by single crystal X-ray diffraction analysis.</p><h3>Index Abstract</h3>\u0000 <div><figure><div><div><picture><source><img></source></picture></div><div><p>The crystal structure of the most stable polymorph of nicotinamide riboside chloride (NR-Cl) is reported.</p></div></div></figure></div>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 4","pages":"465 - 474"},"PeriodicalIF":0.8,"publicationDate":"2023-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48422812","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":"Dynamic Study of Cyclic-Open Tautomerism in a Warfarin Analog","authors":"Edward Danielyan,&nbsp;Maayan Zuniga,&nbsp;Khoi Hoang,&nbsp;David H. Magers,&nbsp;Daniel A. Osborne,&nbsp;Edward J. Valente","doi":"10.1007/s10870-023-00984-2","DOIUrl":"10.1007/s10870-023-00984-2","url":null,"abstract":"<div><p>The more polar product of the Michael addition of 4-hydroxycoumarin to mesityl oxide, an analog of warfarin, crystallizes as the racemic cyclic coumarin hemiketal 2-hydroxy-2,4,4-trimethyl-3,4-dihydro-2<b>H</b>,5<b>H</b>-pyrano[3,2-c][1] benzopyran-5-one. Crystals occur in the monoclinic system, space group <i>P</i>2(1)/<i>n</i>, with <i>a</i> 6.6655(4)Å, <i>b</i> 12.9450(7)Å, <i>c</i> 14.5809(7)Å, <i>β</i> 97.909(5)°, Z = 4. In solution by nuclear magnetic resonance (400 MHz), a dynamic equilibrium exists between the enantiomeric coumarin hemiketals through an unobserved intermediate open tautomer. Diastereomeric methylene and methyl Hs exchange slowly in non-polar solvents (acetic acid and chloroform), much faster in polar, aprotic solvents (acetone and dimethylsulfoxide). In methanol, dynamic behavior begins in the slow-exchange region at 288–310 K, with signal coalescence at 310.5 K, followed by fast-exchange behavior. The barrier to cyclic-open-cyclic (racemization) was found to be ΔG^‡ = + 63(1) kJ/mol (in CD₃OD), with a racemization rate of 30 s⁻¹ at 298 K, 155 s⁻¹ at 310.5 K. Density functional theory (DFT) computations modelling the open and cyclic coumarin tautomers, including solvent fields, confirms that the open-form is 60–70 kJ/mol higher in energy than the cyclic hemiketal. Additionally, modelling supports the contention that chromone tautomers are insignificant participators in solution. An operative <i>gem</i>-dimethyl effect, supported by the proximity of the methyls to the coumarin carboxy oxygen, apparently favors rotamers that bring the side-chain ketone into proximity with the coumarin enolic hydroxy. The less-polar by-product of the Michael addition has been characterized by spectroscopy and crystallography as 2,2,4-trimethyl[2<b>H</b>,5<b>H</b>]pyrano[3,2-c][1]benzopyran-5-one. Computations on the alkyl warfarin analog 2-hydroxy-2,4-dimethyl-3,4-dihydro-2<b>H</b>,5<b>H</b>-pyrano[3,2-c] [1]benzopyran-5-one, lacking the <i>gem</i>-dimethyl effect significantly stabilizes the intermediate open coumarin form, which accords with open-form observations in solution for this analog and for warfarin reported in the literature.</p><h3>Graphical Abstract</h3>\u0000 <div><figure><div><div><picture><img></picture></div></div></figure></div>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 4","pages":"453 - 464"},"PeriodicalIF":0.8,"publicationDate":"2023-05-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42721341","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":"2,4,8,10-Tetra-tert-butyl-6-phenyldibenzo[d,g]-[1,3,6,2]dioxaselena-phosphocine Complexes: C–Se Bond Cleavage and Its Oxidative Addition to Form a Novel Octahedral Rhodium(III) Complex and Hirshfeld Analysis","authors":"Dipanjan Mondal,&nbsp;Pawan Kumar,&nbsp;Joel T. Mague,&nbsp;Maravanji S. Balakrishna","doi":"10.1007/s10870-023-00983-3","DOIUrl":"10.1007/s10870-023-00983-3","url":null,"abstract":"<div><p>Selenaphosphocine [(–OC₆H₂(^<i>t</i>Bu)₂(<i>µ</i>-Se)(^<i>t</i>Bu)₂C₆H₂O–)PhP] (<b>1</b>) on treatment with [Pd(COD)Cl₂] yielded P,Se-coordinated complex [{(–OC₆H₂(^<i>t</i>Bu)₂(<i>µ</i>-Se)(^<i>t</i>Bu)₂C₆H₂O–)PhP}(PdCl₂)] (<b>2</b>), whereas the reaction of <b>1</b> with [AuCl⋅SMe₂] resulted in only P-coordinated complex [{(–OC₆H₂(^<i>t</i>Bu)₂(<i>µ</i>-Se)(^<i>t</i>Bu)₂C₆H₂O–)PhP}(AuCl)] (<b>4</b>). The reaction of <b>1</b> with [Rh(CO)₂Cl]₂ in 4:1 molar ratio yielded a rare Rh^III octahedral complex [{PhP(–OC₆H₂(^<i>t</i>Bu)₂(<i>µ</i>-Se)(^<i>t</i>Bu)₂C₆H₂O–)}{PPh(–OC₆H₂(^<i>t</i>Bu)₂)(Se(^<i>t</i>Bu)₂C₆H₂O–)}(RhCl)] (<b>3</b>) in good yield, in which one of the C–Se bonds of selenophosphocine is added oxidatively to Rh^I. All of the complexes have been structurally characterized and are crystallized in the triclinic crystal system with <i>P</i>¯1 space group. All complexes showed intermolecular C–H⋯O and C–H ⋯Se hydrogen bonding interactions, that play major role in the crystal packing to form a three-dimensional array. In complex <b>2</b>, the crystal packing reveals the presence of rare intermolecular Pd⋯Cl interactions. Hirshfeld surface analysis, d_norm and two-dimensional fingerprint plots were investigated to validate the contributions of the different intermolecular contacts within the supramolecular structure. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of <b>2</b> are from H⋯H (66.3%), C⋯H/H⋯C (13.5%), Cl⋯H/H⋯Cl (13.7%), Cl⋯C/C⋯Cl (1.8%) and Cl⋯C/C⋯Cl (1.0%) contacts, and those for <b>3</b> are from H⋯H (88.3%), C⋯H/H⋯C (8.3%) and Se⋯H/H⋯Se (3.6%) contacts, while those for <b>4</b> are from H⋯H (71.5%), C⋯H/H⋯C (9.9%), Cl⋯H/H⋯Cl (10.2%), Se⋯H/H⋯Se (2.7%) and Au⋯H/H⋯Au (1.7%) contacts.</p><h3>Graphical Abstract</h3><p>This paper describes the cleavage of a C–Se from dioxaselenaphosphocine and its oxidative addition to rhodium(I) complex and Hirshfeld analysis.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"438 - 452"},"PeriodicalIF":0.8,"publicationDate":"2023-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4715624","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 X-ray Structures of 2- and 3-Sulfolene and Two Halogenated Derivatives","authors":"R. Alan Aitken,&nbsp;Alexandra M. Z. Slawin,&nbsp;Dheirya K. Sonecha","doi":"10.1007/s10870-023-00982-4","DOIUrl":"10.1007/s10870-023-00982-4","url":null,"abstract":"<div><p>The structures of the isomeric 2,5-dihydrothiophene 1,1-dioxide [orthorhombic, <i>a</i> = 11.340(2), <i>b</i> = 7.0887(15), <i>c</i> = 6.2811(13) Å, space group <i>Pnma</i>] and 2,3-dihydrothiophene 1,1-dioxide [orthorhombic, <i>a</i> = 6.3903(13), <i>b</i> = 7.2783(16), <i>c</i> = 11.075(2) Å, space group <i>Pnma</i>] have been determined and show perfectly planar rings with the expected bond lengths and angles. In contrast, the halogenated derivatives 3,3,4,4-tetrachlorotetrahydrothiophene 1,1-dioxide [monoclinic, <i>a</i> = 11.8716(8), <i>b</i> = 6.5579(4), <i>c</i> = 11.4802(8) Å, <i>β</i> = 97.705(17), space group <i>P</i>2₁/c] and 2,3-dibromotetrahydrothiophene 1,1-dioxide [orthorhombic, <i>a</i> = 5.2502(3), <i>b</i> = 11.3561(6), <i>c</i> = 24.9802(17) Å, space group <i>Pbca</i>] both show twisted conformations. The degree of planarity is compared with that in the structures of comparable 5-membered ring cyclic sulfones and C–H…O hydrogen bonding patterns are discussed for all four structures.</p><h3>Graphical Abstract</h3><p>The two isomeric sulfolenes are perfectly planar while tetrachloro- and dibromo-derivatives adopt twisted structures.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"431 - 437"},"PeriodicalIF":0.8,"publicationDate":"2023-03-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-023-00982-4.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5122519","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":"Synthetic, Structural and Supramolecular Features of a New Dithiocyanato-κ-N, κ-S-Copper(II) Complex: Insights Through Computational Studies","authors":"Samit Pramanik,&nbsp;Pulak Chandra Mandal,&nbsp;Kinsuk Das,&nbsp;Sudipta Pathak,&nbsp;Subrata Mukhopadhyay","doi":"10.1007/s10870-023-00981-5","DOIUrl":"10.1007/s10870-023-00981-5","url":null,"abstract":"<div><p>A new heterocyclic ligand, <b>L</b> [4-(1-methylimidazole)-2,6-di(pyrazinyl)pyridine] has been synthesized and characterized by adequate spectroscopic methods. The title ligand (<b>L</b>) was then utilized for synthesizing a new complex, namely, [Cu(<b>L</b>)(NCS)(SCN)]·H₂O (complex <b>1</b>) and crystallographically characterised by single-crystal X-ray analysis. In the solid state, the complex unit is stabilized through various hydrogen bonding interactions along with π···π stacking and lone pair···π interactions that lead the molecules to generate diverse supramolecular architectures. Interestingly, the complex exhibits weak S···S interaction which has significant contribution in the solid state crystal packing. All the intermolecular interactions that are involved within the structure are quantified through Hirshfeld surface analyses and confirmed by Bader’s theory of ‘atoms-in-molecules’ (AIM). Finally, an interaction energy analysis was carried out to study the interactions between pairs of molecules.</p><h3>Graphical Abstract</h3><p>The present article reports the synthesis, structural elucidation mentioning the role of supramolecular interactions (π···π stacking, lone pair···π and S···S interactions) and theoretical rationalization [quantified through Hirshfeld surface analyses and confirmed by Bader’s theory of ‘atoms-in-molecules’ (AIM)] of a new dithiocyanato-κ-N, κ-S-copper (II) complex derived from heterocyclic ligand, 4-(1-methylimidazole)-2,6-di(pyrazinyl)pyridine.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"417 - 430"},"PeriodicalIF":0.8,"publicationDate":"2023-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-023-00981-5.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4940977","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":"Synthesis, Structural Characterization and Fluorescent Property of Cd(II) Coordination Polymer Containing Pyridinium Zwitterionic Ligand","authors":"Kaimin Wang,&nbsp;Yanqiu Dong,&nbsp;Xiong Zhao,&nbsp;Xuling Bai,&nbsp;Keyan Duan,&nbsp;Yanqing Ye,&nbsp;Jinrong Guo,&nbsp;Zhengliang Wang,&nbsp;Huaijun Tang,&nbsp;Yulu Ma","doi":"10.1007/s10870-023-00980-6","DOIUrl":"10.1007/s10870-023-00980-6","url":null,"abstract":"<div><p>A novel Cd(II) Coordination Polymer, [Cd(L)₂(SO₄)₂(H₂O)₂][Cd(H₂O)₆]·4H₂O (CP <b>1</b>) (L = (1,1'-((2,3,5,6-tetramethyl-1,4-phenylene)bis(methylene))bis(4-carboxypyridin-1-ium)chloride)), is prepared and characterized by single-crystal X-ray diffraction, elemental analysis, powder X-ray diffraction, infrared spectrum, thermogravimetric analysis, solid-state fluorescence properties and CIE analysis. The single-crystal X-ray diffraction studies reveal that the ligand HLClO₄·H₂O crystallizes in the monoclinic <i>P2</i>_<i>1</i><i>/n</i> space group, while CP <b>1</b> crystallized in the triclinic <i>P-1</i> space group with two distinct Cd(II) centers<i>.</i> Abundant hydrogen bonds produce the 3D supramolecular structure of CP <b>1</b>. The experimental results show that the CP <b>1</b> has good thermal stability and has potential applications in blue luminescent materials.</p><h3>Graphical Abstract</h3><p>The single crystal of a novel Cd (II) coordination polymer based on pyridinium zwitterionic ligand were synthesized in this work.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"407 - 416"},"PeriodicalIF":0.8,"publicationDate":"2023-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4689669","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 Methyl 3-O-α-d-Glucopyranosyl 2-Acetamido-2-Deoxy-α-d-Galactopyranoside Hydrate","authors":"Lars Eriksson,&nbsp;Göran Widmalm","doi":"10.1007/s10870-023-00979-z","DOIUrl":"10.1007/s10870-023-00979-z","url":null,"abstract":"<div><p>Methyl 3-<i>O</i>-α-<span>d</span>-glucopyranosyl 2-acetamido-2-deoxy-α-<span>d</span>-galactopyranoside as a monohydrate, C₁₅H₂₇NO₁₁·H₂O, crystallizes in space group P2₁2₁2₁, with four molecules in the unit cell. It constitutes the methyl glycoside of the carbohydrate part of the teichoic acid type polysaccharide from <i>Micrococcus</i> sp. A1, in which the disaccharides are joined through phosphodiester linkages. The conformation of the disaccharide is described by the glycosidic torsion angles ϕ =  − 31° and ψ =  + 1°, and the hydroxymethyl groups of the constituent monosaccharides are present in the <i>gg</i> and <i>gt</i> conformations for the sugar residues having the <i>gluco</i>- and <i>galacto</i>-configuration, respectively. For the <i>N</i>-acetyl group at C2 of the galactosamine residue the torsion angle τ_H = 147°, i.e., the amide proton has an antiperiplanar relationship to H2 of the sugar ring. The structure shows extensive hydrogen bonding along the a-direction, including the water molecule, and forms sheets with hydrophilic interactions within the sheets as a result of hydrogen bonding between disaccharides as well as hydrophobic interactions between the sheets, in particular, amongst methyl groups of the <i>N</i>-acetyl group of the α-<span>d</span>-Gal<i>p</i>NAc residue in the disaccharides.</p><h3>Graphical Abstract</h3><p>The structure of the title disaccharide as a monohydrate, C₁₅H₂₇NO₁₁·H₂O, which shows extensive hydrogen bonding as well as hydrophobic interactions, was determined from minute crystals using synchrotron radiation and verified by solid state DFT calculations using plane waves.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"400 - 406"},"PeriodicalIF":0.8,"publicationDate":"2023-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-023-00979-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4471719","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":"Synthesis, Structure, Hirshfeld Surface Analysis, Non-Covalent Interaction, and In Silico Studies of 4-Hydroxy-1-[(4-Nitrophenyl)Sulfonyl]Pyrrolidine-2-Carboxyllic Acid","authors":"David Izuchukwu Ugwu,&nbsp;Florence Uchenna Eze,&nbsp;Chigozie Julius Ezeorah,&nbsp;Lydia Rhyman,&nbsp;Ponnadurai Ramasami,&nbsp;Groutso Tania,&nbsp;Cosmas Chinweike Eze,&nbsp;Chiamaka Peace Uzoewulu,&nbsp;Blessing Chinweotito Ogboo,&nbsp;Obinna Chibueze Okpareke","doi":"10.1007/s10870-023-00978-0","DOIUrl":"10.1007/s10870-023-00978-0","url":null,"abstract":"<div><p>The new compound 4-hydroxy-1-[(4-nitrophenyl)sulfonyl]pyrrolidine-2-carboxyllic acid was obtained by the reaction of 4-hydroxyproline with 4-nitrobenzenesulfonyl chloride. The compound was characterized using single crystal X-ray diffraction studies. Spectroscopic methods including NMR, FTIR, ES-MS, and UV were employed for further structural analysis of the synthesized compound. The title compound was found to have crystallized in an orthorhombic crystal system with space group P2₁2₁2₁. The S1-N1 bond length of 1.628 (2) Å was a strong indication of the formation of the title compound. The absence of characteristic downfield ¹H NMR peak of pyrrolidine ring and the presence of S–N stretching vibration at 857.82 cm⁻¹ on the FTIR are strong indications for the formation of the sulfonamide. The experimental study was complemented with computations at the B3LYP/6-311G +  + (d,p) level of theory to gain more understanding of interactions in the compound at the molecular level. Noncovalent interaction, Hirsfeld surface analysis and interaction energy calculations were employed in the analysis of the supramolecular architecture of the compound. Predicted ADMET parameters, awarded suitable bioavailability credentials, while the molecular docking study indicated that the compound enchants promising inhibition prospects against dihydropteroate synthase, DNA topoisomerase, and SARS-CoV-2 spike.\u0000</p><h3>Graphical Abstract</h3><p>Herein we present the solid state structure, noncovalent interaction and spectroscopic analysis of a prospective bioactive compound 4-hydroxy-1-[(4-nitrophenyl)sulphonyl]pyrrolidine-2-carboxyllic acid.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"386 - 399"},"PeriodicalIF":0.8,"publicationDate":"2023-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-023-00978-0.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4395489","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":"The Structure of N-(Chloromethyl)Strychninium Chloride, a Spontaneously Crystallized Product Relevant to Analytical Chemistry, Bioprospecting, and Chiral Separations","authors":"Chloe M. Taylor,&nbsp;Nathan L. Kilah","doi":"10.1007/s10870-022-00977-7","DOIUrl":"10.1007/s10870-022-00977-7","url":null,"abstract":"<div><p>Strychnine is well known as a highly toxic alkaloid derived from the plant <i>Strychnos nux-vomica</i>. It has been applied for chiral separations as a resolving agent for co-crystallizations, as a standard for chromatographic separations, as a rodenticide, as a natural therapy and stimulant, and as a poisonous plot device in works of fiction. Dissolving strychnine into the common organic solvent dichloromethane results in the spontaneous crystallization of the title compound <i>N</i>-(chloromethyl)strychninium chloride. Crystals of the compound were isolated in the orthorhombic space group <i>P</i>2₁2₁2₁ with <i>a</i> = 7.6819(2) Å, <i>b</i> = 7.9621(2) Å, <i>c</i> = 30.7170(9) Å, α = 90°, β = 90°, γ = 90°. The crystal structure has bilayers of <i>N</i>-(chloromethyl)strychninium cations with corresponding bilayers of chloride ions interacting to the cations through C–H hydrogen bonds.</p><h3>Graphical Abstract</h3>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"379 - 385"},"PeriodicalIF":0.8,"publicationDate":"2023-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4212173","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, Hirshfeld Analyses, Spectral, Thermal, Two-Photon Absorption Properties and Optical Limiting Applications of Novel 4-Fluoro-N-[4-(diethylamino)benzylidene]aniline (FDEABA)","authors":"A. Subashini,&nbsp;Reji Philip,&nbsp;Helen Stoeckli-Evans,&nbsp;K. Ramamurthi,&nbsp;R. Ramesh Babu","doi":"10.1007/s10870-022-00975-9","DOIUrl":"10.1007/s10870-022-00975-9","url":null,"abstract":"<div><p>The novel third-order nonlinear optical organic material 4-fluoro-<i>N</i>-[4-(diethylamino)benzylidene]aniline (FDEABA) is synthesized and single crystals of FDEABA are grown using the slow evaporation method. The placement of the protons is confirmed by nuclear magnetic resonance spectral analysis. Employing Fourier transform infrared spectral analysis, vibrational frequencies of various functional groups of the FDEABA compound are identified. The three-dimensional crystal structure of the grown crystal is elucidated using single crystal X-ray diffraction studies, which reveal that the compound FDEABA crystallized in the monoclinic non-centrosymmetric space group P2₁. Intermolecular interactions are studied using Hirshfeld surface analysis and compared with similar structures of halogen-substituted benzylideneaniline derivatives. Thermal stability of FDEABA is measured using thermogravimetric and differential thermal analyses and the melting point of the synthesized FDEABA compound is 51 °C. Open aperture Z-scan measurements carried out at 532 nm using 5 ns laser pulses reveal nonlinear optical absorption leading to strong optical limiting behaviour, which can be useful in the protection of eyes and sensitive optical detectors from harmful laser radiation.</p><h3>Graphical Abstract</h3>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"370 - 378"},"PeriodicalIF":0.8,"publicationDate":"2022-12-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4923332","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}