Acta Crystallographica Section C Structural Chemistry最新文献

{"title":"Diprotonation of taurine: 2-[dihydroxy(oxo)sulfanyliumyl]ethanaminium bis[hexafluoroarsenate(V)].","authors":"Valentin Bockmair, Andreas Klöck, Dirk Hollenwäger, Andreas J Kornath","doi":"10.1107/S2053229624010489","DOIUrl":"10.1107/S2053229624010489","url":null,"abstract":"<p><p>Taurine is part of the cysteine cycle and is one of the few naturally occuring organosulfur-based molecules in the human body. As implied by modern studies, protonated taurine is of biological impact. The first attempts to isolate its protonated species in the binary superacidic system HF/SbF₅ were performed by Hopfinger, resulting in the isolation of monoprotonated taurine. Since the chosen conditions seemed rather harsh, investigations in less acidic systems were performed at room temperature to explore the involved protonated species. Herein, we present the structure of 2-[dihydroxy(oxo)sulfanyliumyl]ethanaminium bis[hexafluoridoarsenate(V)], [H₂O₃SC₂H₄NH₃][AsF₆]₂, the diprotonated form of 2-aminoethanesulfonic acid (taurine). It was synthesized in the binary superacidic system HF/AsF₅ and crystallizes as colourless needles. Diprotonated taurine was structurally characterized by single-crystal X-ray diffraction analysis, low-temperature vibrational spectroscopy and NMR spectroscopy.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"781-786"},"PeriodicalIF":0.7,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11619780/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142674811","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":"Protonated oxalyl chloride and the ClCO⁺ cation.","authors":"Sebastian Steiner, Kristina Djordjevic, Valentin Bockmair, Dirk Hollenwäger, Andreas J Kornath","doi":"10.1107/S2053229624010714","DOIUrl":"10.1107/S2053229624010714","url":null,"abstract":"<p><p>The reactions of oxalyl chloride were investigated in the binary superacidic systems HF/SbF₅ and DF/SbF₅. O-Monoprotonated oxalyl chloride was isolated and represents the first example of a protonated acyl chloride. Diprotonated oxalyl chloride is only stable in solution. Salts of the ClCO⁺ cation were synthesized from the reactions of oxalyl chloride or COClF with SbF₅ in 1,1,1,2-tetrafluoroethane (R-134a, CF₃CFH₂). The colourless salts were characterized by low-temperature vibrational spectroscopy, NMR spectroscopy and single-crystal X-ray diffraction. (1,2-Dichloro-2-oxoethylidene)oxidanium hexafluoridoantimonate(V), [C₂O(OH)Cl₂][SbF₆], crystallizes in the monoclinic space group P2₁ and carbonyl chloride hexadecafluoridotriarsenate(V) [ClCO][Sb₃F₁₆], in the trigonal space group P3₁, with two and three formula units per unit cell, respectively. Monoprotonated oxalyl chloride and the ClCO⁺ cation both display very short C-Cl bonds with a strong double-bond character.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"792-797"},"PeriodicalIF":0.7,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11619778/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142674813","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":"A polymeric form of basic iron(III) acetate with an acetic acid ligand.","authors":"Brendan F Abrahams, Richard Robson, Christopher J Commons","doi":"10.1107/S2053229624010672","DOIUrl":"10.1107/S2053229624010672","url":null,"abstract":"<p><p>A new crystalline compound, catena-poly[hexa-μ-acetato-(acetic acid)-μ₃-oxido-triangulo-triiron(III)]-μ-acetato], [Fe₃(C₂H₃O₂)₇O(C₂H₄O₂)]_n, incorporating the basic ferric acetate unit, has been obtained from an acetic anhydride solution of hydrated iron(III) nitrate. The crystals have the composition Fe₃O(OAc)₇(HOAc) (HOAc is acetic acid) and include the well-known [Fe₃O(OAc)₆]⁺ unit, in which the Fe^III centres are linked to a central coplanar μ₃-oxido ligand. Acetate ions provide bridges between pairs of Fe^III centres. These individual [Fe₃O(OAc)₆]⁺ units are linked by additional bridging acetate anions to form zigzag chains. The bridging acetate ions coordinate to a position trans to the oxido group on two of the Fe^III centres. Remarkably, the trans site on the third Fe^III centre is occupied by the carbonyl group of an acetic acid molecule. This is the first reported case of an acetic acid molecule coordinating to an Fe^III centre. Not surprisingly, the acetic acid molecule is only weakly coordinating, resulting in a short Fe-O(oxido) bond trans to the carbonyl group. The trans influence apparent in this structure provides an interesting contrast with the structurally similar Mn^III analogue, in which the corresponding pair of trans bonds are both elongated because of the Jahn-Teller effect.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"787-791"},"PeriodicalIF":0.7,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142674810","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":"A novel layered structure of the heterometallic oxalate compound [NH₂(CH₃)₂]₂[NaFe(C₂O₄)₃]·0.33NH(CH₃)₂·0.33H₂O: synthesis, crystal structure and thermal decomposition.","authors":"Hamza Kherfi, Mohamed Al Amine Benhacine, Malika Hamadene","doi":"10.1107/S2053229624011185","DOIUrl":"10.1107/S2053229624011185","url":null,"abstract":"<p><p>The synthesis, single-crystal X-ray structure determination and thermal analysis are reported for a novel heteronuclear oxalate compound synthesized from a mixture of Fe and Na salts, oxalic acid and N,N-dimethylformamide (DMF) in aqueous solution. The new metallooxalate compound was obtained and identified as a dimethylammonium tris(oxalato)ferrate(III), namely, poly[[bis(dimethylammonium) [tri-μ-oxalato-sodium(I)iron(III)]]-dimethylamine-water (3/1/1)], [NH₂(CH₃)₂]₂[NaFe(C₂O₄)₃]·0.33NH(CH₃)₂·0.33H₂O, which crystallizes in the orthorhombic noncentrosymmetric space group C222₁. In this novel structure, each Fe atom is hexacoordinated by three non-equivalent bidentate oxalate ligands, while the four Na atoms adopt different coordination numbers, i.e. 6, 7 and 8. The structure consists of bimetallic anionic A layers, {[NaFe(C₂O₄)₃]^2-}_n, displaying a layered structure with infinitely linked Fe₂Na₂ tetramers on the ab plane. Two kinds of bimetallic parallel layers (A1 and A2) are present alternately and are found to be staggered, while only the A2 layer is crossed by a twofold axis parallel to the a axis through two Na atoms. The [NH₂(CH₃)₂]⁺ (HDMA) cations occupy the voids between the anionic layers, while the free molecules, i.e. NH(CH₃)₂ (DMA) and H₂O, are located between two different anionic layers. In addition to ionic bonds, the stability of the structure is ensured by hydrogen-bond interactions involving the oxalate ligands and the nitrogenous and water molecules. The layered structure appears to be different in the family of oxalate-bridged Na^I-Fe^III compounds. It is in agreement with the predicted 2D or layered structure of bimetallic complexes containing anionic tris(oxalato)metallate(III) with the [XR₄]⁺ counter-ion template (X = N, P or S, and R = alkyl group or H). The thermal decomposition of the compound shows the final residual product to be NaFeO₂.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"798-805"},"PeriodicalIF":0.7,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142708535","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":"Construction of pyridine-functionalized metal-organic frameworks for the detection of flazasulfuron.","authors":"Xiaoya Zhao, Boya Su, Qian Zhao, Wan Lv, Litong Chen, Lixin Huang, Xia Li, Shengyun Liao","doi":"10.1107/S2053229624011082","DOIUrl":"10.1107/S2053229624011082","url":null,"abstract":"<p><p>Two novel Cu-based metal-organic frameworks (MOFs), namely, poly[[aquadichlorido[μ₄-4'-(pyridin-4-yl)-[2,2':6',2''-terpyridine]-4,4''-dicarboxylato][μ₃-4'-(pyridin-4-yl)-[2,2':6',2''-terpyridine]-4,4''-dicarboxylato]tricopper(II)] monohydrate], {[Cu₃(C₂₂H₁₂N₄O₄)₂Cl₂(H₂O)]·H₂O}_n or {[Cu₃(PTP)₂Cl₂(H₂O)]·H₂O}_n, (I), and poly[[diaquabis[μ₂-4'-(pyridin-3-yl)-[2,2':6',2''-terpyridine]-4,4''-dicarboxylato]bis(μ₂-terephthalato)tricopper(II)] dihydrate], {[Cu₃(C₂₂H₁₂N₄O₄)₂(C₈H₄O₄)₂(H₂O)₂]·2H₂O}_n or {[Cu₃(BDC)₂(MTP)₂(H₂O)₂]·2H₂O}_n, (II), have been synthesized successfully with 4'-(pyridin-4-yl)-[2,2':6',2''-terpyridine]-4,4''-dicarboxylic acid (H₂PTP) and 4'-(pyridin-3-yl)-[2,2':6',2''-terpyridine]-4,4''-dicarboxylic acid (H₂MTP) as the ligands, respectively. Crystal structure analysis reveals that (II) possesses a 2D coordinated layer structure, in which adjacent 2D coordination layers are linked into 3D frameworks through π-π interactions, while the structure of (I) displays dual coordination layers, in which adjacent coordination layers are connected into a 3D framework through hydrogen-bonding interactions. The photophysical properties of the two MOFs were investigated by fluorescence spectroscopy. Complex (II) shows an obvious `turn-on' fluorescence enhancement effect towards flazasulfuron and its potential application for sensing flazasulfuron in water with high selectivity and sensitivity was also investigated in detail.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"806-814"},"PeriodicalIF":0.7,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142738020","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":"Eu³⁺-doped bismuth silicate crystal structure and Mulliken charge analysis.","authors":"Yan Zhang, Xuefeng Xiao, Yan Huang, Jiashun Si, Shuaijie Liang, Qingyan Xu, Huan Zhang, Lingling Ma, Cui Yang, Xuefeng Zhang, Jiayue Xu, Tian Tian, Hui Shen","doi":"10.1107/S2053229624011410","DOIUrl":"10.1107/S2053229624011410","url":null,"abstract":"<p><p>The effects of Eu³⁺ doping on the crystal structure and charge distribution of Bi₄Si₃O₁₂ (BSO) bisilicate, based on first principles and density functional theory (DFT), were calculated and analyzed using Materials Studio software. The effect of different proportions (1/12, 1/6 and 1/3) of Eu³⁺ doping on BSO crystals was investigated using the virtual crystal approximation method. Through Mulliken charge analysis, it is found that a high proportion of Eu³⁺ doping will destroy the symmetry of the crystal structure. With an increase of the Eu³⁺-doping ratio, the Eu-O bond length first increased and then decreased, showing the characteristics of covalent bonds, and the Eu-O bond length reached the minimum value when the Eu³⁺-doping ratio was increased to 1/3. With an increase in the Eu³⁺-doping ratio, the Bi-O bond length decreases sequentially and also reaches the minimum value when the Eu³⁺-doping ratio was increased to 1/3. This indicates that the covalence between the Eu-O and Bi-O atoms is enhanced when the doping ratio is 1/3 when BSO crystals are doped with Eu³⁺.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"815-820"},"PeriodicalIF":0.7,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142738022","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":"High-throughput crystallization and crystal structure of N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-methylbenzamide: a benzamide bearing the 4-aminoantipyrine moiety.","authors":"Hamad H Al Mamari, Shamsaa Al Sulaimi, Lina Mardiana, Paul G Waddell, Michael J Hall","doi":"10.1107/S2053229624010982","DOIUrl":"10.1107/S2053229624010982","url":null,"abstract":"<p><p>A recent communication on Ru-catalyzed C-H bond arylation with 4-aminoantipyrine (AP) reported the synthesis of AP benzamides. In order to provide additional support to the published structures of AP benzamides, crystallization by high-throughput (HTP) encapsulated nanodroplet crystallization (ENaCt) was undertaken. This allowed for conclusive structure determination by single-crystal X-ray diffraction analysis (SCXRD). This article describes the crystallization and X-ray crystal structure of N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-methylbenzamide, C₁₉H₁₉N₃O₂, as a benzamide bearing 4-aminoantipyrine, providing structural confirmation. X-ray structure analysis reveals intermolecular hydrogen-bonding interactions between the AP benzamide N-H proton and the carbonyl O atom of the AP moiety.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"775-780"},"PeriodicalIF":0.7,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142674812","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":"Bonding properties and crystal packing in β-(SeCl₄)₄ derived from Hirshfeld Atom Refinement.","authors":"Juan de Dios Guzmán-Hernández, Vojtech Jancik","doi":"10.1107/S2053229624010428","DOIUrl":"10.1107/S2053229624010428","url":null,"abstract":"<p><p>Binary chalcogen halogen EX₄ species represent intriguing systems in terms of chemical bonding theories, such as hypervalency and stereoactivity of lone electron pairs. Instead of a simple molecular EX₄ structure, selenium tetrachloride forms an ionic pair, Cl₃Se⁺Cl^-, that assembles into a tetrameric (SeCl₄)₄ structure, namely, tetra-μ₃-chlorido-dodecachloridotetraselenium. This article describes the charge-density analysis of the tetrameric molecule of β-SeCl₄ based on the aspherical model obtained from Hirshfeld Atom Refinement of the tetrameric molecule and of an explicit cluster of 15 tetramers that simulates the crystal packing. Deformation density, electron localization function (ELF) and Quantum Theory of Atoms in Molecules (QTAIM) were used to evaluate the bonding situation, the electron-density distribution around the Se atom and the interaction energy of the tetramer.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"766-774"},"PeriodicalIF":0.7,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11619779/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142612003","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":"Molecular and crystal structures of six poly(arylsulfinyl)- and poly(arylsulfanyl)ferrocenes.","authors":"Tobias Blockhaus, Karlheinz Sünkel","doi":"10.1107/S2053229624009318","DOIUrl":"10.1107/S2053229624009318","url":null,"abstract":"<p><p>Starting from (p-tolylsulfinyl)ferrocene (1), a mixture of the complete series [CpFe{C₅H_5-n(SOTol-p)_n}] (n = 2-4) (2-4) in all regioisomers was obtained. After chromatographic separation, crystals of 1,2-bis[(4-methylbenzene)sulfinyl]ferrocene, 2a, and 1,3-bis[(4-methylbenzene)sulfinyl]ferrocene, 2b, both [Fe(C₅H₅)(C₁₉H₁₇O₂S₂)], as well as of 1,2,3-tris[(4-methylbenzene)sulfinyl]ferrocene, [Fe(C₅H₅)(C₂₆H₂₃O₃S₃)], 3a, and 1,2,3,4-tetrakis[(4-methylbenzene)sulfinyl]ferrocene ethyl acetate 0.75-solvate, [Fe(C₅H₅)(C₃₃H₂₉O₄S₄)]·0.75C₄H₈O₂, 4, could be isolated. Their molecular and crystal structures are compared with each other and also with the so far unreported structures of related 1,2-bis(phenylsulfanyl)ferrocene, [Fe(C₅H₅)(C₁₇H₁₃S₂)], 5, and 1,2,3,4-tetrakis(phenylsulfanyl)ferrocene, [Fe(C₅H₅)(C₂₉H₂₁S₄)], 6. In all the sulfinyl structures, the O atoms of the S=O groups are in equatorial positions, except for that in tetrasubstituted 4. All the arene rings of these compounds (except for one ring in 4) are in axial positions directed away from the Fe atom, mostly in a near perpendicular orientation with respect to the plane of the cyclopentadienyl ring. The main intermolecular interactions in the crystals are C-H...H-C, C-H...π and C-H...O, while C-H...S interactions are much less important, except for tetrasulfanyl compound 6. π-π interactions (intramolecular) are only important in compound 3a. Hirshfeld analysis shows that dispersion terms are dominant for the interaction energies of all six compounds. In general, the calculated total interaction energies increase with increasing number of substituents and are higher for the sulfinyl than for the sulfanyl groups.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"716-727"},"PeriodicalIF":0.7,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11535883/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142370718","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 clear: the impact of crystal structure in the development of high-performance organic semiconductors.","authors":"Callum J McHugh","doi":"10.1107/S2053229624010520","DOIUrl":"https://doi.org/10.1107/S2053229624010520","url":null,"abstract":"","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":"80 Pt 11","pages":"696-697"},"PeriodicalIF":0.7,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142574986","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}