Acta Crystallographica Section C Structural Chemistry最新文献

{"title":"Coordination structure and intermolecular interactions in copper(II) acetate complexes with 1,10-phenanthroline and 2,2'-bipyridine.","authors":"Samuel P Guimaraes, Leonardo H R Dos Santos, Bernardo L Rodrigues","doi":"10.1107/S2053229624007617","DOIUrl":"10.1107/S2053229624007617","url":null,"abstract":"<p><p>The crystal structures of two coordination compounds, (acetato-κO)(2,2'-bipyridine-κ²N,N')(1,10-phenanthroline-κ²N,N')copper(II) acetate hexahydrate, [Cu(C₂H₃O₂)(C₁₀H₈N₂)(C₁₂H₈N₂)](C₂H₃O₂)·6H₂O or [Cu(bipy)(phen)Ac]Ac·6H₂O, and (acetato-κO)bis(2,2'-bipyridine-κ²N,N')copper(II) acetate-acetic acid-water (1/1/3), [Cu(C₂H₃O₂)(C₁₀H₈N₂)₂](C₂H₃O₂)·C₂H₄O₂·3H₂O or [Cu(bipy)₂Ac]Ac·HAc·3H₂O, are reported and compared with the previously published structure of [Cu(phen)₂Ac]Ac·7H₂O (phen is 1,10-phenanthroline, bipy for 2,2'-bipyridine, ac is acetate and Hac is acetic acid). The geometry around the metal centre is pentacoordinated, but highly distorted in all three cases. The coordination number and the geometric distortion are both discussed in detail, and all complexes belong to the space group P-1. The analysis of the geometric parameters and the Hirshfeld surface properties d_norm and curvedness provide information about the metal-ligand interactions in these complexes and allow comparison with similar systems.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"505-513"},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142034924","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-Diarylpyrroles: synthesis, characterization and crystallographic insights.","authors":"Mónica Farfán-Paredes, Rosa Santillan","doi":"10.1107/S2053229624007277","DOIUrl":"10.1107/S2053229624007277","url":null,"abstract":"<p><p>Three 2,4-diarylpyrroles were synthesized starting from 4-nitrobutanones and the crystal structures of two derivatives were analysed. These are 4-(4-methoxyphenyl)-2-(thiophen-2-yl)-1H-pyrrole, C₁₅H₁₃NOS, and 3-(4-bromophenyl)-2-nitroso-5-phenyl-1H-pyrrole, C₁₆H₁₁BrN₂O. Although pyrroles without substituents at the α-position with respect to the N atom are very air sensitive and tend to polymerize, we succeeded in growing an adequate crystal for X-ray diffraction analysis. Further derivatization using sodium nitrite afforded a nitrosyl pyrrole derivative, which crystallized in the triclinic space group P-1 with Z = 6. Thus, herein we report the first crystal structure of a nitrosyl pyrrole. Interestingly, the co-operative hydrogen bonds in this NO-substituted pyrrole lead to a trimeric structure with bifurcated halogen bonds at the ends, forming a two-dimensional (2D) layer with interstitial voids having a radius of 5 Å, similar to some reported macrocyclic porphyrins.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"472-477"},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141900525","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":"Formation of a diiron-(μ-η¹:η¹-CN) complex from acetonitrile solution.","authors":"Tim P Schlachta, Michael J Sauer, Leon F Richter, Fritz E Kühn","doi":"10.1107/S2053229624007058","DOIUrl":"10.1107/S2053229624007058","url":null,"abstract":"<p><p>The activation of C-C bonds by transition-metal complexes is of continuing interest and acetonitrile (MeCN) has attracted attention as a cyanide source with comparatively low toxicity for organic cyanation reactions. A diiron end-on μ-η¹:η¹-CN-bridged complex was obtained from a crystallization experiment of an open-chain iron-NHC complex, namely, μ-cyanido-κ²C:N-bis{[(acetonitrile-κN)[3,3'-bis(pyridin-2-yl)-1,1'-(methylidene)bis(benzimidazol-2-ylidene)]iron(II)} tris(hexafluorophosphate), [Fe₂(CN)(C₂H₃N)₂(C₂₅H₁₈N₆)₂](PF₆)₃. The cyanide appears to originate from the MeCN solvent by C-C bond cleavage or through carbon-hydrogen oxidation.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"534-537"},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11370999/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141900527","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 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":" ","pages":"538-544"},"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":"Crystal structures, phase transition, and Hirshfeld surface analyses of the bromide and chloride congeners of aqua[2,4,6-tris(pyridin-4-yl)-1,3,5-triazine]zinc(II) halide.","authors":"Maegan Dailey, Eric W Jackson, Timothy R Ramadhar","doi":"10.1107/S205322962400737X","DOIUrl":"10.1107/S205322962400737X","url":null,"abstract":"<p><p>During the course of exploring crystallization conditions in generating metal-organic frameworks (MOFs) for use in the crystalline sponge method, two discrete metal-organic complexes, namely, aqua[2,4,6-tris(pyridin-4-yl)-1,3,5-triazine]zinc(II) bromide, [Zn(C₁₈H₁₂N₆)(H₂O)]Br₂, and aqua[2,4,6-tris(pyridin-4-yl)-1,3,5-triazine]zinc(II) chloride, [Zn(C₁₈H₁₂N₆)(H₂O)]Cl₂, were encountered. Structures in the orthorhombic space group Pnma (No. 62) for the bromide congener at 299 K and the chloride congener at 100 K were obtained. A phase transition for the bromide congener occurred upon cooling from 299 to 100 K, yielding a crystal polymorph with four domains that exhibits monoclinic P2₁/m space-group symmetry (No. 11), which arises from conformational changes. The main intramolecular contacts that contribute to the crystal packing in all observed structures are H...H, Halide...H/H...Halide, C...H/H...C, and N...H/H...N. Intramolecular hydrogen bonding between the Zn-bound water and non-Zn-bound pyridyl N atoms is a prominent feature within the three-dimensional networks. Aromatic π-stacking between the non-Zn-bound pyridine rings and contacts involving the halide ligands further stabilize the crystal packing.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"545-552"},"PeriodicalIF":0.7,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141915861","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":" ","pages":"576-583"},"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":"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":" ","pages":"448-449"},"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":"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":" ","pages":"450-457"},"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":"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":" ","pages":"458-471"},"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":"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":" ","pages":"514-522"},"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}