Acta Crystallographica Section C Structural Chemistry最新文献_第5页

Where are the lone pairs? QC and QCT. 孤对在哪里？QC和QCT。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2025-02-01 Epub Date: 2025-01-06 DOI: 10.1107/S2053229624012488

Fernando Cortés-Guzmán

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Structural investigations of benzoyl fluoride and the benzoacyl cation of low-melting compounds and reactive intermediates. 低熔点化合物和活性中间体中苯甲酰氟和苯甲酰阳离子的结构研究。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2025-02-01 Epub Date: 2025-01-24 DOI: 10.1107/S2053229625000476

Valentin Bockmair, Martin Regnat, Huu Khanh Trinh Tran, Andreas J Kornath

{"title":"Structural investigations of benzoyl fluoride and the benzoacyl cation of low-melting compounds and reactive intermediates.","authors":"Valentin Bockmair, Martin Regnat, Huu Khanh Trinh Tran, Andreas J Kornath","doi":"10.1107/S2053229625000476","DOIUrl":"10.1107/S2053229625000476","url":null,"abstract":"Acyl fluorides and acyl cations represent typical reactive intermediates in organic reactions, such as Friedel-Crafts acylation. However, the comparatively stable phenyl-substituted compounds have not been fully characterized yet, offering a promising backbone. Attempts to isolate the benzoacylium cation have only been carried out starting from the acyl chloride with weaker chloride-based Lewis acids. Therefore, only adducts of 1,4-stabilized acyl cations could be obtained. Due to the low melting point of benzoyl fluoride, together with its volitality and sensitivity toward hydrolysis, the structures of the acyl fluoride and its acylium cation have not been determined. Herein, we report the first crystal structure of benzoyl fluoride, C7H5FO or PhCOF (monoclinic P21/n, Z = 8) and the benzoacylium undecafluorodiarsenate, C7H5O+·As2F11- or [PhCO]+[As2F11]- (monoclinic P21/n, Z = 4). The compounds were characterized by low-temperature vibrational spectroscopy and single-crystal X-ray analysis, and are discussed together with quantum chemical calculations. In addition, their specific π-interactions were elucidated.","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"93-101"},"PeriodicalIF":0.7,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11795653/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143031732","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

Monoprotonated species of 2-aminomalonyl difluoride, [C₃H₄F₂NO₂][H₂F₃]. [C3H4F2NO2][H2F3]的单质子化种。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2025-02-01 Epub Date: 2025-01-08 DOI: 10.1107/S2053229624012452

Dirk Hollenwäger, Dominik Leitz, Valentin Bockmair, Andreas J Kornath

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Synthesis and diverse crystal packing in o-, m- and p-bis(carbonylthioureido)benzenes containing bisferrocenes. 含二茂铁的o-、m-和对-双（羰基硫脲）苯的合成和不同的晶体填充。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2025-02-01 Epub Date: 2025-01-23 DOI: 10.1107/S2053229625000282

Xin E Duan, Ze Jin Jiang, Hong Bo Tong, Sheng Di Bai

{"title":"Synthesis and diverse crystal packing in o-, m- and p-bis(carbonylthioureido)benzenes containing bisferrocenes.","authors":"Xin E Duan, Ze Jin Jiang, Hong Bo Tong, Sheng Di Bai","doi":"10.1107/S2053229625000282","DOIUrl":"10.1107/S2053229625000282","url":null,"abstract":"Three bisferrocene-based bis(acylthiourea) positional isomers, namely, 1,2-bis(ferrocenylcarbonylthioureido)benzene (1), 1,3-bis(ferrocenylcarbonylthioureido)benzene (2) and 1,4-bis(ferrocenylcarbonylthioureido)benzene (3), all [Fe2(C5H5)2(C20H16N4O2S2)], have been synthesized via facile nucleophilic addition reactions of 2.3 equivalents of ferrocenoyl isothiocyanate with o-, m- and p-phenylenediamine, respectively. The structures of the three new synthesized isomers were fully characterized by 1H NMR, 13C NMR, IR and UV-Vis spectroscopy, elemental analyses and cyclic voltammetry. In addition, the structures of acetone monosolvated compound 1 (1·CH3COCH3), as well as compounds 2 and 3, have been determined by single-crystal X-ray diffraction. A combination of intermolecular N-H...S and C-H...S hydrogen bonds connects the components of compound 1·CH3COCH3 into infinite helix chains. Two pairs of different N-H...S and C-H...S intermolecular hydrogen bonds, as well as N-H...O and C-H...π co-operating interactions, link the molecules of compound 2 into a two-dimensional network. In contrast, compound 3 displays a one-dimensional double-chain array via two intermolecular C-H...S hydrogen bonds. Therefore, the three reported positional isomers present unique individual crystal assemblies.","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"82-92"},"PeriodicalIF":0.7,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143021618","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}

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The crystal structures of methyl prop-2-ynoate, dimethyl fumarate and their protonated species. 2-醋酸丙酸甲酯、富马酸二甲酯及其质子化产物的晶体结构。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2025-01-01 DOI: 10.1107/S2053229624011653

Dirk Hollenwäger, Valentin Bockmair, Andreas J Kornath

{"title":"The crystal structures of methyl prop-2-ynoate, dimethyl fumarate and their protonated species.","authors":"Dirk Hollenwäger, Valentin Bockmair, Andreas J Kornath","doi":"10.1107/S2053229624011653","DOIUrl":"10.1107/S2053229624011653","url":null,"abstract":"Methyl prop-2-ynoate (C4H4O2) was investigated in the binary superacidic system HF/MF5 (M = Sb or As) and dimethyl fumarate (C6H8O4) in the superacidic system HF/SbF5, as well as HF/BF3. The starting materials methyl prop-2-ynoate and dimethyl fumarate were crystallized, the former for the first time. The protonated species of these esters, namely, (1-methoxyprop-2-yn-1-ylidene)oxidanium hexafluoroarsenate, C4H5O2+ AsF6-, 1,4-dimethoxy-4-oxobut-2-en-1-ylidene]oxidanium tetrafluoroborate bis(hydrogen fluoride), C6H9O4+ BF4- 2HF, and hemi{[1,4-dimethoxy-4-oxidaniumylidenebut-2-en-1-ylidene]oxidanium} undecafluorodiantimonate, 0.5C6H10O42+ Sb2F11-, were characterized by single-crystal X-ray diffraction and Raman spectroscopy. The protonated species were recrystallized from anhydrous hydrogen fluoride. In the solid state of the monoprotonated species of methyl prop-2-ynoate and the diprotonated species of dimethyl fumarate, strong intramolecular O-H...F hydrogen bonds build a three-dimensional network. The monoprotonated species of dimethyl fumarate builds chains by strong O-H...O hydrogen bonds between the cations.","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"31-37"},"PeriodicalIF":0.7,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142798966","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

How to use DIALS to process chemical crystallography 3D ED rotation data from pixel array detectors. 如何使用DIALS处理来自像素阵列探测器的化学晶体学3D ED旋转数据。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2025-01-01 DOI: 10.1107/S2053229624011148

Angelina Vypritskaia, Xiaodong Zou, Taimin Yang, David Geoffrey Waterman

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Crown ether inclusion compound 3,4-difluoroanilinium di(methanesulfonyl)amidate-18-crown-6 (1/1) clathrate. 冠醚包合物 3,4-二氟苯胺二(甲磺酰基)酰胺-18-冠-6 (1/1) 凝块。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2025-01-01 DOI: 10.1107/S2053229624011872

Yao Zhang, Yan Juan Wang, Yuan Yuan Tang, Xiao Gang Chen

{"title":"Crown ether inclusion compound 3,4-difluoroanilinium di(methanesulfonyl)amidate-18-crown-6 (1/1) clathrate.","authors":"Yao Zhang, Yan Juan Wang, Yuan Yuan Tang, Xiao Gang Chen","doi":"10.1107/S2053229624011872","DOIUrl":"10.1107/S2053229624011872","url":null,"abstract":"In recent years, molecular-based ferroelectric materials have attracted widespread research interest due to their excellent performance. Among them, host-guest-type crown ether inclusion compounds composed of organic ammonium cations, crown ether molecules and corresponding anions have become a star component in the design of molecular-based ferroelectric materials because they are prone to order-disorder phase transitions. Many anions have been studied extensively as counter-ions, such as bis(trifluoromethanesulfonyl)amidate (TFSA-), PF6- and [FeCl4]-. However, crown ether inclusion compounds with di(methanesulfonyl)amidate (DMSA) as the anion have been rarely investigated. Here, we converted TFSA to DMSA to obtain 3,4-difluoroanilinium di(methanesulfonyl)amidate-18-crown-6 (1/1), C6H6F2N+·C2H6NO4S2-·C12H24O6 or [(3,4-DFA)(18-crown-6)][DMSA]. At both 100 and 300 K, the crystal falls into the space group P21/c. The 3,4-DFA cation forms three well-defined N-H...O hydrogen bonds, positioned at the perching position of the crown ether ring. In contrast to the distinct packing configuration observed in the [(3,4-DFA)(18-crown-6)][TFSA] crystals, where TFSA exhibits a disordered structure, the [(3,4-DFA)(18-crown-6)][DMSA] complex features a staggered arrangement, with DMSA existing in an ordered fashion.","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"38-42"},"PeriodicalIF":0.7,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142833421","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}

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A personal account of the history of X-ray crystallography at the University of La Plata, Argentina. 阿根廷拉普拉塔大学x射线晶体学历史的个人叙述。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2025-01-01 DOI: 10.1107/S2053229624011495

Oscar Enrique Piro

{"title":"A personal account of the history of X-ray crystallography at the University of La Plata, Argentina.","authors":"Oscar Enrique Piro","doi":"10.1107/S2053229624011495","DOIUrl":"10.1107/S2053229624011495","url":null,"abstract":"Prompted by visionary political leaders and a flowering economy, the University of La Plata was founded in 1905, the third Argentinian university after the Universities of Cordoba (1613) and Buenos Aires (1821). Differing from the older universities, more prone to professional formation, the new university was oriented towards teaching and scientific research following western European academic tradition. Along with the university was created the Institute of Physics, the first of its kind in Latin America. To pursue the foundational plan, the university recruited distinguished German physicists, some of whom became the first directors. From the start, the institute became acquainted with Röntgen rays, their generation and use, initially for radiographic images and later in occasional diffraction studies. The first dedicated crystallographic X-ray diffraction laboratory was set up in the early 1970s, when it solved the first molecular structures. Soon the fascination brought about by a methodology that afforded the visualization of atoms, molecules and crystals lured the local and national physical chemistry communities. In close partnership with an equally oriented laboratory at the University of Sao Paulo, Brazil, and in collaboration with several physical chemistry laboratories from Argentina and the Latin American region, and also from Europe, we undertook studies on the crystal structures and physicochemical and spectroscopic properties of a wide range of materials, including inorganic, organic, bioinorganic, metal-organic, organic-metal, supramolecular, pharmaceutical, organic minerals and liquid crystals. The present essay is a personal account of the origin and development of structural X-ray crystallography at the University of La Plata and its impact on the scientific research of Argentina and Latin America.","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"14-21"},"PeriodicalIF":0.7,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142783563","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

Diprotonation of taurine: 2-[dihydroxy(oxo)sulfanyliumyl]ethanaminium bis[hexafluoroarsenate(V)]. 牛磺酸的二质子化作用：2-[二羟基（氧代）硫铵基]乙铵双[六氟砷酸盐（V）]。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2024-12-01 Epub Date: 2024-11-20 DOI: 10.1107/S2053229624010489

Valentin Bockmair, Andreas Klöck, Dirk Hollenwäger, Andreas J Kornath

{"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":"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.","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}

引用次数: 0

Protonated oxalyl chloride and the ClCO⁺ cation. 质子化草酰氯和 ClCO+ 阳离子。

IF 0.7 4区化学

Acta Crystallographica Section C Structural Chemistry Pub Date : 2024-12-01 Epub Date: 2024-11-20 DOI: 10.1107/S2053229624010714

Sebastian Steiner, Kristina Djordjevic, Valentin Bockmair, Dirk Hollenwäger, Andreas J Kornath

{"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":"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.","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}

引用次数: 0