Acta Crystallographica Section E: Crystallographic Communications最新文献

Crystal structure of bis(diisopropylamino)fluoroborane 双（二异丙基氨基）氟硼烷的晶体结构。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025003160

Tabea Lenz , Marian Hebenbrock

引用次数: 0

Crystal structure and Hirshfeld surface analysis of the fungicide metconazole 杀菌剂美康唑的晶体结构及赫氏表面分析。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S205698902500310X

Thaluru M. Mohan Kumar , Chaluvarangaiah Sowbhagya , Hemmige S. Yathirajan , Sean Parkin

{"title":"Crystal structure and Hirshfeld surface analysis of the fungicide metconazole","authors":"Thaluru M. Mohan Kumar , Chaluvarangaiah Sowbhagya , Hemmige S. Yathirajan , Sean Parkin","doi":"10.1107/S205698902500310X","DOIUrl":"10.1107/S205698902500310X","url":null,"abstract":"<div><div>The crystal structure of [(1<em>S</em>,5<em>R</em>)/(1<em>R</em>,5<em>S</em>)]-<em>cis</em>-metconazole at 100 K is presented along with a Hirshfeld surface analysis comparing the similarities of the atom–atom contacts involving the two independent molecules in the asymmetric unit.</div></div><div><div>Metconazole is a systemic triazole fungicide that inhibits the ergosterol biosynthesis pathway. It is widely used in agriculture to control fungal infections, including rusts, fusarium and septoria diseases. The molecular structure is a three-ring system, namely, 5-(4-chlorobenzyl)-2,2-dimethyl-1-(1<em>H</em>-1,2,4-triazol-1-ylmethyl)cyclopentan-1-ol, C<sub>17</sub>H<sub>22</sub>ClN<sub>3</sub>O, consisting of a cyclopentan-1-ol with 1,2,4-triazol-1-ylmethyl, <em>gem</em>-dimethyl and 4-chlorobenzyl groups attached at the 1-, 2- and 5-positions of the cyclopentanol ring. It has two stereocentres (cyclopentanol positions 1 and 5) leading to four stereoisomers, with the (1<em>S</em>,5<em>R</em>) form being the most bioactive. Despite its agricultural significance, detailed crystallographic data remain scarce. This study reports the crystal structure and Hirshfeld surface analysis of racemic <em>cis</em>-metconazole [(1<em>S</em>,5<em>R</em>)/(1<em>R</em>,5<em>S</em>)], determined in the monoclinic space group <em>P</em>2<sub>1</sub>/<em>c</em> with two independent molecules in the asymmetric unit (<em>Z</em>′ = 2). Both exhibit similar conformations, with minor differences in the cyclopentanol ring puckering and the torsion angles between the three rings. The crystal packing consists of 2<sub>1</sub>-screw-related hydrogen-bonded chains parallel to the <em>b</em> axis, with additional weak C—H⋯N and C—H⋯Cl contacts linking adjacent molecules. Hirshfeld surface analysis indicates that intermolecular interactions are dominated by contacts involving hydrogen (96.1 and 96.7% for the two molecules).</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 385-388"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143956247","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Di-μ3-chlorido-1:2:3κ3Cl;2:3:4κ3Cl-di-μ2-chlorido-1:2κ2Cl;3:4κ2Cl-tetrakis[(4-amino-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one-κ2N4,O)chloridocadmium(II)] 1.7-hydrate: a new six-coordinate geometry index, τ6 [（4-氨基-1,5-二甲基-2-苯基-2,3-二氢- 1h -吡唑-3- 1 -κ2 N，O）氯-镉（II）] 1.7-水合物：一个新的六坐标几何指数τ6。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025003123

Helen Stoeckli-Evans , M. G. Shankar , R. Kumaravel , A. Subashini , T. Sabari Girisun , K. Ramamurthi , Monika Kučeráková , Michal Dušek , Aurélien Crochet

{"title":"Di-μ3-chlorido-1:2:3κ3Cl;2:3:4κ3Cl-di-μ2-chlorido-1:2κ2Cl;3:4κ2Cl-tetrakis[(4-amino-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one-κ2N4,O)chloridocadmium(II)] 1.7-hydrate: a new six-coordinate geometry index, τ6","authors":"Helen Stoeckli-Evans , M. G. Shankar , R. Kumaravel , A. Subashini , T. Sabari Girisun , K. Ramamurthi , Monika Kučeráková , Michal Dušek , Aurélien Crochet","doi":"10.1107/S2056989025003123","DOIUrl":"10.1107/S2056989025003123","url":null,"abstract":"<div><div>A new tetranuclear cadmium(II) complex of 4-aminoantipyrine and chloride ions was synthesized using methanol as solvent. The complex possesses inversion symmetry with two independent Cd<sup>2+</sup> ions that have different coordination spheres, one fivefold and the other sixfold. A new geometry index, τ<sub>6</sub>, is propossed to quantitatively describe the geometry of a sixfold coordinated atom.</div></div><div><div>The title centrosymmetric tetranuclear cadmium(II) complex of 4-aminoantipyrine and chloride ions, [Cd<sub>4</sub>Cl<sub>8</sub>(C<sub>11</sub>H<sub>13</sub>N<sub>3</sub>O)<sub>4</sub>]·1.7H<sub>2</sub>O, was synthesized using methanol as solvent. The two independent Cd<sup>2+</sup> ions in the asymmetric unit have different geometries; the outer Cd atoms have fivefold CdONCl<sub>3</sub> coordination spheres, while the inner Cd atoms have sixfold CdONCl<sub>4</sub> coordination spheres. The complex is consolidated by intramolecular N—H⋯O and N—H⋯Cl hydrogen bonds. In the crystal, a combination of N—H⋯Cl and O<sub>w</sub>—H⋯Cl (w = water) hydrogen bonds link the components to form chains propagating along the <em>a</em>-axis direction. The chains are crosslinked by C—H⋯Cl and C—H⋯O hydrogen bonds to form a three-dimensional structure. A new geometry index, τ<sub>6</sub>, is proposed to quantitatively estimate the geometry of a sixfold coordinated atom.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 393-400"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143955843","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Synthesis and structure of 4-bromo-2-chlorophenyl 4′-methoxy-[1,1′-biphenyl]-4-carboxylate featuring short halogen⋯oxygen contacts 具有短卤素⋯氧接触的4-溴-2-氯苯基4'-甲氧-[1,1'-联苯基]-4-羧酸盐的合成和结构。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025002658

B. S. Palakshamurthy , H. Anil Kumar , H. C. Devarajegowda , H.T. Srinivasa , M. Harish Kumar

{"title":"Synthesis and structure of 4-bromo-2-chlorophenyl 4′-methoxy-[1,1′-biphenyl]-4-carboxylate featuring short halogen⋯oxygen contacts","authors":"B. S. Palakshamurthy , H. Anil Kumar , H. C. Devarajegowda , H.T. Srinivasa , M. Harish Kumar","doi":"10.1107/S2056989025002658","DOIUrl":"10.1107/S2056989025002658","url":null,"abstract":"<div><div>The extended structure features short halogen⋯oxygen contacts [Cl⋯O = 2.991 (3), Br⋯O = 3.139 (2) Å], forming molecular sheets lying parallel to (101).</div></div><div><div>In the title compound, C<sub>20</sub>H<sub>14</sub>BrClO<sub>3</sub>, the dihedral angles between the aromatic ring of the 4-bromo-2-chlorophenyl and the immediate neighbour and second aromatic ring of the biphenyl moiety are 80.59 (2) and 75.42 (2)°, respectively. The dihedral angle between the rings within the biphenyl moiety is 24.57 (4)°. The torsion angle associated with the ester group linking the biphenyl ring and the 4-bromo-2-chlorophenyl group is −166.6 (2)°. The extended structure features short halogen⋯oxygen contacts [Cl⋯O = 2.991 (3), Br⋯O = 3.139 (2) Å], forming molecular sheets lying parallel to (101). The Hirshfeld surface analysis reveals that the major contributions to the intermolecular interactions are from C⋯H/H⋯C (32.2%), H⋯H/H⋯H (26.3%), Br⋯H/H⋯Br (10.7%), O⋯H/H⋯O (10.4%) and Cl⋯H/H⋯Cl (7.5%) contacts.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 364-367"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143956274","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

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Orthosilicates with glaserite-type crystal structures: Na2BaZr[SiO4]2 and Na2BaHf[SiO4]2 具有glaserite型晶体结构的正硅酸盐：Na2BaZr[SiO4]2和Na2BaHf[SiO4]2。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025002956

Hisanori Yamane , Shiro Funahashi , Naoto Hirosaki , Takashi Takeda

{"title":"Orthosilicates with glaserite-type crystal structures: Na2BaZr[SiO4]2 and Na2BaHf[SiO4]2","authors":"Hisanori Yamane , Shiro Funahashi , Naoto Hirosaki , Takashi Takeda","doi":"10.1107/S2056989025002956","DOIUrl":"10.1107/S2056989025002956","url":null,"abstract":"<div><div>The two title oxides are new isotypic silicates, crystallizing in the non-centrosymmetric space group <em>P</em>3. The crystal structures were analysed with two twin components in each case.</div></div><div><div>Single crystal particles of Na<sub>2</sub>BaZr[SiO<sub>4</sub>]<sub>2</sub> [systematic name: disodium barium zirconium bis(orthosilicate)] and Na<sub>2</sub>BaHf[SiO<sub>4</sub>]<sub>2</sub> [disodium barium hafnium bis(orthosilicate)] were extracted from grain-grown polycrystals obtained by heating compacts of binary oxide mixtures at 1473 K. Single crystal X-ray diffraction analysis revealed that these are isostructural orthosilicates with a glaserite-type crystal structure, in which all sites of <em>X</em>, <em>Y</em>, <em>M</em>, and <em>T</em> in the general formula <em>XY</em><sub>2</sub>[<em>M</em>(<em>T</em>O<sub>4</sub>)<sub>2</sub>] are fully occupied by atoms of different elements. The crystal structures of the title compounds were refined in space group <em>P</em>3 under consideration of a two-component twin model. The SiO<sub>4</sub> tetrahedra are rotated approximately ±10.2° from the mirror plane of space group <em>P</em>3<em>m</em> around an axis parallel to [001].</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 368-371"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143963194","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Synthesis, crystal structure and Hirshfeld surface analysis of 2,2-dichloro-3,3-diethoxy-1-(4-fluorophenyl)propan-1-ol 2,2-二氯-3,3-二eth-氧-1-（4-氟苯基）丙烷-1-醇的合成、晶体结构和Hirshfeld表面分析。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025002154

Saadet N. Guseynova , Aida I. Samigullina , Cemile Baydere Demir , Necmi Dege , Nayim Sepay , Ennio Zangrando , Khudayar I. Hasanov , Alebel N. Belay

{"title":"Synthesis, crystal structure and Hirshfeld surface analysis of 2,2-dichloro-3,3-diethoxy-1-(4-fluorophenyl)propan-1-ol","authors":"Saadet N. Guseynova , Aida I. Samigullina , Cemile Baydere Demir , Necmi Dege , Nayim Sepay , Ennio Zangrando , Khudayar I. Hasanov , Alebel N. Belay","doi":"10.1107/S2056989025002154","DOIUrl":"10.1107/S2056989025002154","url":null,"abstract":"<div><div>We have isolated and structurally chracterized 2,2-dichloro-3,3-diethoxy-1-(4-fluorophenyl)propan-1-ol by simple hydrogenation of 2,2-dichloro-3,3-diethoxy-1-(4-fluorophenyl)propan-1-one. Hirshfeld surface analysis was performed.</div></div><div><div>The title molecule, C<sub>13</sub>H<sub>17</sub>Cl<sub>2</sub>FO<sub>3</sub>, crystallizes in the orthorhombic space group <em>P</em>2<sub>1</sub>2<sub>1</sub>2<sub>1</sub> with one molecule in the asymmetric unit. The skeleton of the molecule exhibits an <em>anti</em> conformation with a C—C—C—C(Ph) torsion angle of −174.97 (18)°. The species are weakly hydrogen bonded to form a polymeric chain elongated in the direction of the <em>b</em> axis. This interaction is realised by the hydroxyl group with an ether O atom of a symmetry-related species [O—H⋯O hydrogen-bond distance of 2.975 (2) Å]. No π-stacking interaction involving the fluorobenzyl moiety is detected in the crystal structure. Hirshfeld surface analysis, confirming the O—H⋯O donor–acceptor interactions, indicates that the most important contributions to the surface contacts are H⋯H (47.0%), Cl⋯H (19.5%), C⋯H (12.1%) and F⋯H (10.7%).</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 444-447"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143959504","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

An Ni-based coordination polymer with a bamboo-like crystal structure 一种具有竹状晶体结构的镍基配位聚合物。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025002993

Yi Li , Wang Xie , Chen Lin

{"title":"An Ni-based coordination polymer with a bamboo-like crystal structure","authors":"Yi Li , Wang Xie , Chen Lin","doi":"10.1107/S2056989025002993","DOIUrl":"10.1107/S2056989025002993","url":null,"abstract":"<div><div>An Ni-based coordination polymer with a crystal structure reminiscent of bamboo has been synthesized, the Ni<sup>2+</sup> ions exhibiting a slightly distorted octahedral coordination geometry with N atoms and O atoms.</div></div><div><div>An Ni-based coordination polymer, namely, poly[tetraaquabis[4,7-bis(1<em>H</em>-pyrazol-4-yl)benzo[<em>c</em>][1,2,5]thiadiazole][μ<sub>4</sub>-5,5′-(1,3,6,8-tetraoxo-1,3,6,8-tetrahydrobenzo[<em>lmn</em>][3,8]phenanthroline-2,7-diyl)diisophthalato]dinickel(II)], {[Ni<sub>2</sub>(C<sub>30</sub>H<sub>10</sub>N<sub>2</sub>O<sub>12</sub>)(C<sub>12</sub>H<sub>8</sub>N<sub>6</sub>S)<sub>2</sub>(H<sub>2</sub>O)<sub>4</sub>]·2C<sub>3</sub>H<sub>7</sub>NO·H<sub>2</sub>O}<sub><em>n</em></sub> or <strong>Ni-BIBT-BINDI</strong>, with a crystal structure reminiscent of bamboo has been synthesized, the Ni<sup>2+</sup> ions exhibiting a slightly distorted octahedral coordination geometry with N atoms and O atoms. The bond lengths of the Ni—O bonds range from 2.032 to 2.121 Å, and those of the Ni—N bonds are approximately 2.080 Å. The BINDI ligands are connected to each other by the Ni—O bonds, which form the backbone of the bamboo, while the BIBT ligands are connected to the backbone of the bamboo through Ni—N bonds and grows on both sides of the bamboo, constituting the bamboo leaves.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 377-380"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143955840","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Structure of (E)-4-amino-5-{[(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)imino]methyl}-1-methyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one: aerial oxidation of 4-aminoantipyrine in dimethylformamide (E)-4-氨基-5-{[（1,5-二甲基-3-氧-2-苯基-2,3-二氢- 1h -吡唑-4-基）亚胺]-甲基}-1-甲基-2-苯基-2,3-二氢- 1h -吡唑-3-酮的结构：二甲基甲酰胺中4-氨基抗吡啶的航空氧化反应。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025003676

R. Kumaravel , Helen Stoeckli-Evans , A. Subashini , M. G. Shankar , Monika Kučeráková , Michal Dušek , Aurélien Crochet , K. Ramamurthi

{"title":"Structure of (E)-4-amino-5-{[(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)imino]methyl}-1-methyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one: aerial oxidation of 4-aminoantipyrine in dimethylformamide","authors":"R. Kumaravel , Helen Stoeckli-Evans , A. Subashini , M. G. Shankar , Monika Kučeráková , Michal Dušek , Aurélien Crochet , K. Ramamurthi","doi":"10.1107/S2056989025003676","DOIUrl":"10.1107/S2056989025003676","url":null,"abstract":"<div><div>The formation of the title compound is best explained by the aerial oxidation of the 5-methyl group of 4-aminoantipyrine to an aldehyde group, and subsequent intermolecular Schiff base formation with a second molecule of 4-aminoantipyrine. The reaction only takes place in the presence of dimethylformamide.</div></div><div><div>The title compound, C<sub>22</sub>H<sub>22</sub>N<sub>6</sub>O<sub>2</sub> (<strong>I</strong>), is the result of the aerial oxidation of the 5-methyl group of 4-aminoantipyrine to an aldehyde group followed by Schiff base formation with a second molecule of 4-aminoantipyrine. The reaction only takes place in the presence of dimethylformamide. The central unit of the molecule is close to planar, the pyrazole rings being inclined to each other by 3.74 (15)°. There is an intramolecular N—H⋯N hydrogen bond enclosing an <em>S</em>(6) ring motif and there are two further <em>S</em>(6) rings involving weak C—H⋯O=C hydrogen bonds. The molecule has an <em>E</em> configuration about the azomethine (—N=CH—) bond. In the crystal, inversion-related molecules are linked by pairs of N—H⋯O hydrogen bonds, forming dimers enclosing <em>R</em><sup>2</sup><sub>2</sub>(10) loops. The dimers are linked by C—H⋯O hydrogen bonds and C—H⋯π interactions, leading to the formation of a three-dimensional supramolecular network.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 438-443"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143955074","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Synthesis and crystal structure of 2-(2,4-dioxo-6-methylpyran-3-ylidene)-4-(4-hydroxyphenyl)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine 2-（2,4-二氧基-6-甲基吡喃-3-基二烯）-4-（4-羟基苯基）-2,3,4,5-四氢- 1h -1,5-苯二氮杂卓的合成与晶体结构

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025003032

Imane Faraj , Lhoussaine El Ghayati , Olivier Blacque , Tuncer Hökelek , Ahmed Mazzah , El Mokhtar Essassi , Nada Kheira Sebbar

{"title":"Synthesis and crystal structure of 2-(2,4-dioxo-6-methylpyran-3-ylidene)-4-(4-hydroxyphenyl)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine","authors":"Imane Faraj , Lhoussaine El Ghayati , Olivier Blacque , Tuncer Hökelek , Ahmed Mazzah , El Mokhtar Essassi , Nada Kheira Sebbar","doi":"10.1107/S2056989025003032","DOIUrl":"10.1107/S2056989025003032","url":null,"abstract":"<div><div>In the crystal, O—H⋯O and N—H⋯O hydrogen bonds link the molecules, enclosing <em>R</em><sub>2</sub><sup>2</sup>(16) and <em>R</em><sub>2</sub><sup>2</sup>(24) ring motifs, to generate [110] chains. Very weak π–π stacking interactions between the phenyl rings of adjacent molecules help to consolidate a three-dimensional architecture.</div></div><div><div>The title compound, C<sub>21</sub>H<sub>18</sub>N<sub>2</sub>O<sub>4</sub>, contains non-planar diazepine (in a boat–sofa conformation) and pyran (envelope) rings. In the crystal, O—H⋯O and N—H⋯O hydrogen bonds link the molecules, enclosing <em>R</em><sub>2</sub><sup>2</sup>(16) and <em>R</em><sub>2</sub><sup>2</sup>(24) ring motifs, to generate [110] chains. Very weak π–π stacking interactions between the phenyl rings of adjacent molecules with an inter-centroid distance of 4.0264 (9) Å help to consolidate a three-dimensional architecture. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (45.1%), H⋯O/O⋯H (23.2%) and H⋯C/C⋯H (19.2%) interactions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 381-384"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143967503","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Synthesis and crystal structure study of (R,R)-TMCDA ethanol derivatives doubly protonated with FeCl4− and Cl− as counter-ions 以FeCl4 -和Cl-为反离子双质子化（R，R）- tmcda乙醇衍生物的合成和晶体结构研究。

IF 0.5

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2025-05-01 DOI: 10.1107/S2056989025003019

Franziska Dorothea Klotz , Clara Alonso Felipe , Fernando Villafañe , Carsten Strohmann

{"title":"Synthesis and crystal structure study of (R,R)-TMCDA ethanol derivatives doubly protonated with FeCl4− and Cl− as counter-ions","authors":"Franziska Dorothea Klotz , Clara Alonso Felipe , Fernando Villafañe , Carsten Strohmann","doi":"10.1107/S2056989025003019","DOIUrl":"10.1107/S2056989025003019","url":null,"abstract":"<div><div>The synthesis and structural characterization of the crystal forms of (<em>R</em>,<em>R</em>)-TMCDA and its ethanol derivative, both doubly protonated with FeCl<sub>4</sub><sup>−</sup> and Cl<sup>−</sup> as counter-ions, are reported. A notable feature across both synthesized compounds is the presence of N—H⋯Cl hydrogen bonds of moderate strength in the solid state. In the case of the ethanol derivative of (<em>R</em>,<em>R</em>)-TMCDA, the structure also reveals the formation of intermolecular O–H⋯Cl hydrogen bonds.</div></div><div><div>The synthesis and structural characterization of the crystal forms of (<em>R</em>,<em>R</em>)-TMCDA and its ethanol derivative, both doubly protonated with FeCl<sub>4</sub><sup>−</sup> and Cl<sup>−</sup> as counter-ions, are reported, namely, (<em>R</em>,<em>R</em>)-<em>N</em><sup>1</sup>,<em>N</em><sup>1</sup>,<em>N</em><sup>2</sup>,<em>N</em><sup>2</sup>-tetramethylcyclohexane-1,2-bis(aminium) tetrachloridoferrate chloride, (C<sub>10</sub>H<sub>24</sub>N<sub>2</sub>)[FeCl<sub>4</sub>]Cl (<strong>1a</strong>), and (<em>R</em>,<em>R</em>)-<em>N</em><sup>1</sup>-(2-hydroxyethyl)-<em>N</em><sup>1</sup>,<em>N</em><sup>2</sup>,<em>N</em><sup>2</sup>-trimethylcyclohexane-1,2-bis(aminium) tetrachloridoferrate chloride (C<sub>11</sub>H<sub>26</sub>N<sub>2</sub>O)[FeCl<sub>4</sub>]Cl (<strong>2a</strong>). A notable feature across both synthesized compounds is the presence of N—H⋯Cl hydrogen bonds of moderate strength in the solid state. In the case of the ethanol derivative of (<em>R</em>,<em>R</em>)-TMCDA, the structure also reveals the formation of intermolecular O—H⋯Cl hydrogen bonds.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 5","pages":"Pages 372-376"},"PeriodicalIF":0.5,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143963706","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

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