Acta Crystallographica Section C Structural Chemistry最新文献

{"title":"A luminescent Cu₂I₂P₂S₂-type binuclear complex and its fluorescence sensing for pyridine.","authors":"Jin Tao Wu, Li Song, Wen Ze Xu, Xin Yu Wei, Yu Xin Zhang, Ying Ying Zhang, Xin Yang Du, Wen Xiang Chai","doi":"10.1107/S2053229624006983","DOIUrl":"10.1107/S2053229624006983","url":null,"abstract":"<p><p>Luminescent Cu^I complexes are an important class of coordination compounds due to their relative abundance, low cost and ability to display excellent luminescence. The title Cu₂I₂P₂S₂-type binuclear complex, di-μ-iodido-bis[(thiourea-κS)(triphenylphosphine-κP)copper(I)], [Cu₂I₂(CH₄N₂S)₂(C₁₈H₁₅P)₂], conventionally abbreviated as Cu₂I₂TPP₂TU₂, where TPP and TU represent triphenylphosphine and thiourea, respectively, is described. In this complex, each Cu^I atom adopts a CuI₂PS four-coordination mode and pairs of atoms are connected to each other by two μ₂-I ligands to form a centrosymmetric binuclear cluster. It was also found that the paper-based film of this complex exhibited obvious luminescence light-up sensing for pyridine and 4-methylpyridine.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141905513","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 challenges of growing great crystals - or at least good enough ones!","authors":"Alexander J Blake","doi":"10.1107/S2053229624008416","DOIUrl":"10.1107/S2053229624008416","url":null,"abstract":"<p><p>The article of Sommer [Acta Cryst. (2024), C80, 337-342] provides a concise and effective introduction to the subject of growing crystals suitable for structure determination.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142071727","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":"Coordination variety of phenyltetrazolato and dimethylamido ligands in dimeric Ti, Zr, and Ta complexes.","authors":"Galina A Bikzhanova, Ilia A Guzei","doi":"10.1107/S2053229624007411","DOIUrl":"10.1107/S2053229624007411","url":null,"abstract":"<p><p>Three structurally diverse 5-phenyltetrazolato (Tz) Ti, Zr, and Ta complexes, namely, (C₂H₈N)[Ti₂(C₇H₅N₄)₅(C₂H₆N)₄]·1.45C₆H₆ or (Me₂NH₂)[Ti₂(NMe₂)₄(2,3-μ-Tz)₃(2-η¹-Tz)₂]·1.45C₆H₆, (1·1.45C₆H₆), [Zr₂(C₇H₅N₄)₆(C₂H₆N)₂(C₂H₇N)₂]·1.12C₆H₆·0.382CH₂Cl₂ or [Zr₂(Me₂NH)₂(NMe₂)₂(2,3-μ-Tz)₃(2-η¹-Tz)₂(1,2-η²-Tz)]·1.12C₆H₆·0.38CH₂Cl₂ (2·1.12C₆H₆·0.38CH₂Cl₂), and (C₂H₈N)₂[Ta₂(C₇H₅N₄)₈(C₂H₆N)₂O]·0.25C₇H₈ or (Me₂NH₂)₂[Ta₂(NMe₂)₂(2,3-μ-Tz)₂(2-η¹-Tz)₆O]·0.25C₇H₈ (3·0.25C₇H₈), where TzH is 5-phenyl-1H-tetrazole, have been synthesized and structurally characterized. All three complexes are dinuclear; the Ti center in 1 is six-coordinate, whereas the Zr and Ta atoms in 2 and 3 are seven-coordinate. The coordination environments of the Ti centers in 1 are similar, and so are the ligations of the Ta centers in 3. In contrast, the two Zr centers in 2 bear a different number of ligands, one of which is a bidentate η²-5-phenyltetrazolato ligand that has not been observed previously for d-block elements. The dimethylamido ligand, present in the starting materials, remained unchanged, or was converted to dimethylamine and dimethylammonium during the synthesis. Dimethylamine coordinates as a neutral ligand, whereas dimethylammonium is retained as a hydrogen-bonded entity bridging Tz ligands.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11371001/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142034939","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":"Dicarbonyl[10,10-dimethyl-5,15-bis(pentafluorophenyl)biladiene]ruthenium(II): discovery of the first ruthenium tetrapyrrole cis-dicarbonyl complex by X-ray and electron diffraction.","authors":"Trong Nhan Pham, Hunter Shirley, Johannes Merkelbach, Kshitij Gurung, Lukáš Palatinus, Glenn P A Yap, Joel Rosenthal","doi":"10.1107/S2053229624007083","DOIUrl":"10.1107/S2053229624007083","url":null,"abstract":"<p><p>Dicarbonyl[10,10-dimethyl-5,15-bis(pentafluorophenyl)biladiene]ruthenium(II), [Ru(C₃₃H₁₆F₁₀N₄)(CO)₂] or Ru(CO)₂[DMBil1], is the first reported ruthenium(II) cis-dicarbonyl tetrapyrrole complex. The neutral complex sports two carbonyls and an oligotetrapyrrolic biladiene ligand. Notably, the biladiene adopts a coordination geometry that is well distorted from square planar and much more closely approximates a seesaw arrangement. Accordingly, Ru(CO)₂[DMBil1] is not only the first ruthenium cis-dicarbonyl with a tetrapyrrole ligand, but also the first metal biladiene complex in which the tetrapyrrole does not adopt a (pseudo-)square-planar coordination geometry. Ru(CO)₂[DMBil1] is weakly luminescent, displaying λ_em = 552 nm upon excitation at λ_ex = 500 nm, supports two reversible 1 e^- reductions at -1.45 and -1.73 V (versus Fc⁺/Fc), and has significant absorption features at 481 and 531 nm, suggesting suitability for photocatalytic and photosensitization applications. While the structure of Ru(CO)₂[DMBil1] was initially determined by X-ray diffraction, a traditionally acceptable quality structure could not be obtained (despite multiple attempts) because of consistently poor crystal quality. An independent structure obtained from electron diffraction experiments corroborates the structure of this unusual biladiene complex.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11371002/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141905514","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":"Salt forms of amides: protonation of acetanilide.","authors":"Harry S Jaconelli, Alan R Kennedy","doi":"10.1107/S2053229624007332","DOIUrl":"10.1107/S2053229624007332","url":null,"abstract":"<p><p>Treating the amide acetanilide (N-phenylacetamide, C₈H₉NO) with aqueous strong acids allowed the structures of five hemi-protonated salt forms of acetanilide to be elucidated. N-(1-Hydroxyethylidene)anilinium chloride-N-phenylacetamide (1/1), [(C₈H₉NO)₂H][Cl], and the bromide, [(C₈H₉NO)₂H][Br], triiodide, [(C₈H₉NO)₂H][I₃], tetrafluoroborate, [(C₈H₉NO)₂H][BF₄], and diiodobromide hemi(diiodine), [(C₈H₉NO)₂H][I₂Br]·0.5I₂, analogues all feature centrosymmetric dimeric units linked by O-H...O hydrogen bonds that extend into one-dimensional hydrogen-bonded chains through N-H...X interactions, where X is the halide atom of the anion. Protonation occurs at the amide O atom and results in systematic lengthening of the C=O bond and a corresponding shortening of the C-N bond. The size of these geometric changes is similar to those found for hemi-protonated paracetamol structures, but less than those in fully protonated paracetamol structures. The bond angles of the amide fragments are also found to change on protonation, but these angular changes are also influenced by conformation, namely, whether the amide group is coplanar with the phenyl ring or twisted out of plane.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11371003/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141900530","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 structures of two unexpected products of vicinal diamines left to crystallize in acetone.","authors":"Bruno Dival, Leonardo Pitinato, Letícia Develly, Willian X C Oliveira","doi":"10.1107/S2053229624007320","DOIUrl":"10.1107/S2053229624007320","url":null,"abstract":"<p><p>Herein we report the crystal structures of two benzodiazepines obtained by reacting N,N'-(4,5-diamino-1,2-phenylene)bis(4-methylbenzenesulfonamide) (1) or 4,5-(4-methylbenzenesulfonamido)benzene-1,2-diaminium dichloride (1·2HCl) with acetone, giving 2,2,4-trimethyl-8,9-bis(4-methylbenzenesulfonamido)-2,3-dihydro-5H-1,5-benzodiazepine, C₂₆H₃₀N₄O₄S₂ (2), and 2,2,4-trimethyl-8,9-bis(4-methylbenzenesulfonamido)-2,3-dihydro-5H-1,5-benzodiazepin-1-ium chloride 0.3-hydrate, C₂₆H₃₁N₄O₄S₂⁺·Cl^-·0.3H₂O (3). Compounds 2 and 3 were first obtained in attempts to recrystallize 1 and 1·2HCl using acetone as solvent. This solvent reacted with the vicinal diamines present in the molecular structures, forming a 5H-1,5-benzodiazepine ring. In the crystal structure of 2, the seven-membered ring of benzodiazepine adopts a boat-like conformation, while upon protonation, observed in the crystal structure of 3, it adopts an envelope-like conformation. In both crystalline compounds, the tosylamide N atoms are not in resonance with the arene ring, mainly due to hydrogen bonds and steric hindrance caused by the large vicinal groups in the aromatic ring. At a supramolecular level, the crystal structure is maintained by a combination of hydrogen bonds and hydrophobic interactions. In 2, amine-to-tosyl N-H...O and amide-to-imine N-H...N hydrogen bonds can be observed. In contrast, in 3, the chloride counter-ion and water molecule result in most of the hydrogen bonds being of the amide-to-chloride and ammonium-to-chloride N-H...Cl types, while the amine interacts with the tosyl group, as seen in 2. In conclusion, we report the synthesis of 1, 1·2HCl and 2, as well as their chemical characterization. For 2, two synthetic methods are described, i.e. solvent-mediated crystallization and synthesis via a more efficient and cleaner route as a polycrystalline material. Salt 3 was only obtained as presented, with only a few crystals being formed.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142034940","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":"Two polymorph modifications of tris(hexafluoroacetylacetonato)iron(III) revealed: is that common for other trivalent metals?","authors":"Joyce Chang, Julianna N Defeo, Zheng Wei, Evgeny V Dikarev","doi":"10.1107/S2053229624007575","DOIUrl":"10.1107/S2053229624007575","url":null,"abstract":"<p><p>A long-standing issue about the correct identification of an important starting reagent, iron(III) hexafluoroacetylacetonate, Fe(hfac)₃ (1), has been resolved. The tris-chelated mononuclear complex was found to crystallize in two polymorph modifications which can be assigned as the low-temperature (1-L) monoclinic P2₁/n and the high-temperature (1-H) trigonal P-3. Low-temperature polymorph 1-L was found to transform to 1-H upon sublimation at 44 °C. Two modifications are clearly distinguished by powder X-ray diffraction (PXRD), single-crystal X-ray diffraction, differential scanning calorimetry (DSC), and melting-point measurements. On the other hand, the two forms share similar characteristics in direct analysis in real-time mass spectrometry (DART-MS), attenuated total reflection (ATR) spectroscopy, and some physical properties, such as color, volatility, sensitivity, and solubility. Analysis of the literature and some of our preliminary data strongly suggest that the appearance of two polymorph modifications for trivalent metal (both transition and main group) hexafluoroacetylacetonates is a common case for several largely used complexes not yet accounted for in the crystallographic databases.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142003367","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 brief review on computer simulations of chalcopyrite surfaces: structure and reactivity.","authors":"Guilherme Randow Nascimento, Selma Fabiana Bazan, Guilherme Ferreira de Lima","doi":"10.1107/S2053229624006867","DOIUrl":"10.1107/S2053229624006867","url":null,"abstract":"<p><p>Chalcopyrite, the world's primary copper ore mineral, is abundant in Latin America. Copper extraction offers significant economic and social benefits due to its strategic importance across various industries. However, the hydrometallurgical route, considered more environmentally friendly for processing low-grade chalcopyrite ores, remains challenging, as does its concentration by froth flotation. This limited understanding stems from the poorly understood structure and reactivity of chalcopyrite surfaces. This study reviews recent contributions using density functional theory (DFT) calculations with periodic boundary conditions and slab models to elucidate chalcopyrite surface properties. Our analysis reveals that reconstructed surfaces preferentially expose S atoms at the topmost layer. Furthermore, some studies report the formation of disulfide groups (S₂^2-) on pristine sulfur-terminated surfaces, accompanied by the reduction of Fe³⁺ to Fe²⁺, likely due to surface oxidation. Additionally, Fe sites are consistently identified as favourable adsorption locations for both oxygen (O₂) and water (H₂O) molecules. Finally, the potential of computer modelling for investigating collector-chalcopyrite surface interactions in the context of selective froth flotation is discussed, highlighting the need for further research in this area.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141900526","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":"Synthesis, structure and red-light emission of a manganese halide directed by a methyldiphenylphosphine oxide complex.","authors":"Jia Wei Li, Mengyuan Niu, Wei Feng, Wenke Dong, Yanjie Liu, Jingjing Yang, Chunjie Wang, Hui Zhang, Wei Wu Song","doi":"10.1107/S2053229624006405","DOIUrl":"10.1107/S2053229624006405","url":null,"abstract":"<p><p>Controlling the optical activity of halide perovskite materials through modulation of the coordination configurations of the metal ions is important. Herein, a novel manganese-based halide, specifically diaquatetrakis(methyldiphenylphosphine oxide)manganese(II) tetrachloridomanganate(II), [Mn(C₁₃H₁₃OP)₄(H₂O)₂][MnCl₄] or [Mn(MDPPO)₄(H₂O)₂][MnCl₄] (MDPPO is methyldiphenylphosphine oxide), was synthesized through the solvothermal reaction of MnCl₂ with the neutral molecule MDPPO. In this compound, [Mn(MDPPO)₄(H₂O)₂]²⁺ acts as the cation, while [MnCl₄]^2- serves as the anion, enabling the co-existence of tetrahedral and octahedral structures within the same system. Remarkably, the compound exhibits efficient red-light emission at 662 nm, distinct from the green-light emission typically observed in MnX₄-based halides. Theoretical calculations show that the red emission comes from the charge transfer from the MDPPO to the Mn²⁺ of [MnCl₄]^2-. This work provides a new perspective for the design and synthesis of red-light-emitting manganese-based halides with unique structures.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141589413","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 and cryomagnetic study of a mononuclear erbium(III) oxamate inclusion complex.","authors":"Cleber R Araujo Junior, Willian X C Oliveira, Carlos B Pinheiro, Emerson F Pedroso, Wallace C Nunes, Adriele A de Almeida, Marcelo Knobel, Miguel Julve, Cynthia L M Pereira","doi":"10.1107/S2053229624005977","DOIUrl":"10.1107/S2053229624005977","url":null,"abstract":"<p><p>The synthesis, crystal structure and magnetic properties of an oxamate-containing erbium(III) complex, namely, tetrabutylammonium aqua[N-(2,4,6-trimethylphenyl)oxamato]erbium(III)-dimethyl sulfoxide-water (1/3/1.5), (C₁₆H₃₆N)[Er(C₁₁H₁₂NO₃)₄(H₂O)]·3C₂H₆OS·1.5H₂O or n-Bu₄N[Er(Htmpa)₄(H₂O)]·3DMSO·1.5H₂O (1), are reported. The crystal structure of 1 reveals the occurrence of an erbium(III) ion, which is surrounded by four N-phenyl-substituted oxamate ligands and one water molecule in a nine-coordinated environment, together with one tetrabutylammonium cation acting as a counter-ion, and one water and three dimethyl sulfoxide (DMSO) molecules of crystallization. Variable-temperature static (dc) and dynamic (ac) magnetic measurements were carried out for this mononuclear complex, revealing that it behaves as a field-induced single-ion magnet (SIM) below 5.0 K.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141562395","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}