The title compound [Fe(C21H13N3S)(CO)(PMe3)2] exhibits a square-pyramidal geometry, distinct from the trigonal–bipyramidal geometry in [Fe(C21H13N3S)(CO)3], due to the σ-donating properties of the two trimethylphosphane ligands. An increase in π-back-donation from the electron-rich iron center to the pyridazine moiety was also confirmed.
The title compound, [Fe(C21H13N3S)(CO)(PMe3)2] (2), bearing a 3-(dibenzo[b,d]thiophen-4-yl)-6-(pyridin-2-yl)pyridazine ligand was obtained by the reaction of [Fe(C21H13N3S)(CO)3] (1) with [Fe(PMe3)4]. Crystal structure analysis of 2 revealed that the N,N-bidentate and three monodentate ligands form a five-coordinate square-pyramidal geometry around Fe, which differs from the trigonal–bipyramidal geometry observed in 1. The steric and electronic factors were investigated by combining crystal structure and density functional theory (DFT) calculations. Compared with CO, the better σ donor properties of PMe3 induce the square-pyramidal geometry of 2, and a significant π-back-bonding interaction was confirmed between Fe and the pyridazine moiety.
{"title":"Synthesis, crystal structure and DFT study of carbonyl[3-(dibenzo[b,d]thiophen-4-yl)-6-(pyridin-2-yl-κN)pyridazine-κN1]bis(trimethylphosphane)iron(0)","authors":"Ryota Futaki , Noriko Chikaraishi Kasuga , Masakazu Hirotsu","doi":"10.1107/S2056989025010953","DOIUrl":"10.1107/S2056989025010953","url":null,"abstract":"<div><div>The title compound [Fe(C<sub>21</sub>H<sub>13</sub>N<sub>3</sub>S)(CO)(PMe<sub>3</sub>)<sub>2</sub>] exhibits a square-pyramidal geometry, distinct from the trigonal–bipyramidal geometry in [Fe(C<sub>21</sub>H<sub>13</sub>N<sub>3</sub>S)(CO)<sub>3</sub>], due to the σ-donating properties of the two trimethylphosphane ligands. An increase in π-back-donation from the electron-rich iron center to the pyridazine moiety was also confirmed.</div></div><div><div>The title compound, [Fe(C<sub>21</sub>H<sub>13</sub>N<sub>3</sub>S)(CO)(PMe<sub>3</sub>)<sub>2</sub>] (<strong>2</strong>), bearing a 3-(dibenzo[<em>b</em>,<em>d</em>]thiophen-4-yl)-6-(pyridin-2-yl)pyridazine ligand was obtained by the reaction of [Fe(C<sub>21</sub>H<sub>13</sub>N<sub>3</sub>S)(CO)<sub>3</sub>] (<strong>1</strong>) with [Fe(PMe<sub>3</sub>)<sub>4</sub>]. Crystal structure analysis of <strong>2</strong> revealed that the <em>N</em>,<em>N</em>-bidentate and three monodentate ligands form a five-coordinate square-pyramidal geometry around Fe, which differs from the trigonal–bipyramidal geometry observed in <strong>1</strong>. The steric and electronic factors were investigated by combining crystal structure and density functional theory (DFT) calculations. Compared with CO, the better σ donor properties of PMe<sub>3</sub> induce the square-pyramidal geometry of <strong>2</strong>, and a significant π-back-bonding interaction was confirmed between Fe and the pyridazine moiety.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 61-66"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963193","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}
Pub Date : 2026-01-01DOI: 10.1107/S205698902501117X
Katsuya Kaikake , Sotaro Kusumoto , Ren-Hua Jin
The crystal structure of a new complex between the theophylline ligand and palladium has been elucidated.
An air-stable palladium bis(benzyltheophylline) complex, [PdCl2(C14H14N4O2)2]·0.5H2O, was synthesized from 7-benzyltheophylline and palladium dichloride. Single-crystal X-ray diffraction analysis revealed that the complex adopts a centrosymmetric structure in which two theophylline ligands coordinate to the square-planar PdII center through N atoms on the imidazole ring. The crystal structure contains water molecules located at partially occupied sites (occupancy = 1/4). A notable structural feature is that the fused purine ring system of each ligand is oriented nearly perpendicular to the square-planar PdII coordination plane. In addition, the pendant phenyl ring is almost perpendicular to the fused purine ring plane, as indicated by the large torsion angle around the C5—N4—C8—C9 linkage [84.1 (2)°]. These geometric characteristics highlight the steric influence exerted by the benzyltheophylline ligand on the metal coordination environment.
{"title":"Crystal structure of trans-bis(7-benzyl-1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione)dichloridopalladium(II) hemihydrate","authors":"Katsuya Kaikake , Sotaro Kusumoto , Ren-Hua Jin","doi":"10.1107/S205698902501117X","DOIUrl":"10.1107/S205698902501117X","url":null,"abstract":"<div><div>The crystal structure of a new complex between the theophylline ligand and palladium has been elucidated.</div></div><div><div>An air-stable palladium bis(benzyltheophylline) complex, [PdCl<sub>2</sub>(C<sub>14</sub>H<sub>14</sub>N<sub>4</sub>O<sub>2</sub>)<sub>2</sub>]·0.5H<sub>2</sub>O, was synthesized from 7-benzyltheophylline and palladium dichloride. Single-crystal X-ray diffraction analysis revealed that the complex adopts a centrosymmetric structure in which two theophylline ligands coordinate to the square-planar Pd<sup>II</sup> center through N atoms on the imidazole ring. The crystal structure contains water molecules located at partially occupied sites (occupancy = 1/4). A notable structural feature is that the fused purine ring system of each ligand is oriented nearly perpendicular to the square-planar Pd<sup>II</sup> coordination plane. In addition, the pendant phenyl ring is almost perpendicular to the fused purine ring plane, as indicated by the large torsion angle around the C5—N4—C8—C9 linkage [84.1 (2)°]. These geometric characteristics highlight the steric influence exerted by the benzyltheophylline ligand on the metal coordination environment.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 82-85"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963253","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}
Bis(4-phenylbutan-2-one-κ2O,O′)copper(II) (P21/n) features an almost ideal square-planar CuO4 core and forms offset chains along [011] consolidated by π–π, weak π–metal and C—H⋯O contacts. Hirshfeld analysis shows dominant H⋯H contacts (54.8%); DFT (UB3LYP, ECP on Cu) gives HOMO/LUMO = −6.19/−1.83 eV (ΔE = 4.36 eV), consistent with mixed MLCT/ligand-centered transitions and high electronic stability.
In the title compound, [Cu(C10H9O2)2], which crystallizes in space group P21/n, the central CuII ion is four-coordinate and closely approaches an ideal square-planar geometry: Cu—O = 1.9173 (18)–1.920 (2) Å, O—Cu—O = 93.34 (7)°, τ4 = 0.00, CShM(square-planar) = 0.085. The crystal packing features offset chains along [011] consolidated by π–π interactions [Cg⋯Cg = 3.1293 (1) Å], weak π–metal contacts [Cg⋯Cu = 3.390 (2) Å], and C—H⋯O contacts; Hirshfeld surface analysis shows dominant H⋯H contacts (54.8%), followed by H⋯C (18.8%) and O⋯H (11.3%). DFT (UB3LYP, ECP on Cu) yields E(HOMO) = −6.19 eV, E(LUMO) = −1.83 eV, ΔE = 4.36 eV; the HOMO has a significant metal contribution while the LUMO is ligand π* in character, indicating mixed metal-to-ligand charge-transfer (MLCT)/ligand-centered transitions and high electronic stability.
{"title":"Synthesis, crystal structure, Hirshfeld surface and DFT analysis of bis(4-oxo-4-phenylbut-2-en-2-olato-κ2O,O′)copper(II)","authors":"Kyzlarkhan Siddikova , Sardor Murodov , Daminbek Ziyatov , Dilafruz Jabbarova , Jamshid Ashurov , Shakhlo Daminova","doi":"10.1107/S2056989025011089","DOIUrl":"10.1107/S2056989025011089","url":null,"abstract":"<div><div>Bis(4-phenylbutan-2-one-κ<sup>2</sup><em>O</em>,<em>O</em>′)copper(II) (<em>P</em>2<sub>1</sub>/<em>n</em>) features an almost ideal square-planar CuO<sub>4</sub> core and forms offset chains along [011] consolidated by π–π, weak π–metal and C—H⋯O contacts. Hirshfeld analysis shows dominant H⋯H contacts (54.8%); DFT (UB3LYP, ECP on Cu) gives HOMO/LUMO = −6.19/−1.83 eV (Δ<em>E</em> = 4.36 eV), consistent with mixed MLCT/ligand-centered transitions and high electronic stability.</div></div><div><div>In the title compound, [Cu(C<sub>10</sub>H<sub>9</sub>O<sub>2</sub>)<sub>2</sub>], which crystallizes in space group <em>P</em>2<sub>1</sub>/<em>n</em>, the central Cu<sup>II</sup> ion is four-coordinate and closely approaches an ideal square-planar geometry: Cu—O = 1.9173 (18)–1.920 (2) Å, O—Cu—O = 93.34 (7)°, τ<sub>4</sub> = 0.00, CShM(square-planar) = 0.085. The crystal packing features offset chains along [011] consolidated by π–π interactions [<em>Cg</em>⋯<em>Cg</em> = 3.1293 (1) Å], weak π–metal contacts [<em>Cg</em>⋯Cu = 3.390 (2) Å], and C—H⋯O contacts; Hirshfeld surface analysis shows dominant H⋯H contacts (54.8%), followed by H⋯C (18.8%) and O⋯H (11.3%). DFT (UB3LYP, ECP on Cu) yields <em>E</em>(HOMO) = −6.19 eV, <em>E</em>(LUMO) = −1.83 eV, Δ<em>E</em> = 4.36 eV; the HOMO has a significant metal contribution while the LUMO is ligand π* in character, indicating mixed metal-to-ligand charge-transfer (MLCT)/ligand-centered transitions and high electronic stability.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 77-81"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963251","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}
Pub Date : 2026-01-01DOI: 10.1107/S2056989025010588
Danylo S. Kreiman , Dmytro M. Korytko , Iryna S. Kuzevanova , Mihaela Dascalu , Il’ya A. Gural’skiy
Bis(2-bromoethanamminium) hexabromidostannate(IV) is a hybrid tin perovskite with 0D topology due to the presence of isolated octahedral [SnBr6]2– anions.
In the hybride title salt, (C2H7BrN)2[SnBr6], the charge of the anionic [SnBr6]2− moiety is balanced by two (H3N(CH2)2Br)+ cations. The tin(IV) atom is located on a mirror plane and has a slightly distorted octahedral coordination environment. The inorganic octahedra are discrete, thus leading to a 0D topology within the crystal structure. The two crystallographically unique organic cations have different conformations: while one has a gauche conformation, the other has an anti conformation, both without special symmetry but with positional disorder over the crystallographic mirror plane. Contacts between organic and inorganic parts in the crystal structure are ensured by N—H⋯Br hydrogen bonds and weak Br⋯Br and C—H⋯Br interactions.
{"title":"Crystal structure of bis(2-bromoethylammonium) hexabromidostannate(IV)","authors":"Danylo S. Kreiman , Dmytro M. Korytko , Iryna S. Kuzevanova , Mihaela Dascalu , Il’ya A. Gural’skiy","doi":"10.1107/S2056989025010588","DOIUrl":"10.1107/S2056989025010588","url":null,"abstract":"<div><div>Bis(2-bromoethanamminium) hexabromidostannate(IV) is a hybrid tin perovskite with 0D topology due to the presence of isolated octahedral [SnBr<sub>6</sub>]<sup>2–</sup> anions.</div></div><div><div>In the hybride title salt, (C<sub>2</sub>H<sub>7</sub>BrN)<sub>2</sub>[SnBr<sub>6</sub>], the charge of the anionic [SnBr<sub>6</sub>]<sup>2−</sup> moiety is balanced by two (H<sub>3</sub>N(CH<sub>2</sub>)<sub>2</sub>Br)<sup>+</sup> cations. The tin(IV) atom is located on a mirror plane and has a slightly distorted octahedral coordination environment. The inorganic octahedra are discrete, thus leading to a 0D topology within the crystal structure. The two crystallographically unique organic cations have different conformations: while one has a <em>gauche</em> conformation, the other has an <em>anti</em> conformation, both without special symmetry but with positional disorder over the crystallographic mirror plane. Contacts between organic and inorganic parts in the crystal structure are ensured by N—H⋯Br hydrogen bonds and weak Br⋯Br and C—H⋯Br interactions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 1-4"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963256","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}
Pub Date : 2026-01-01DOI: 10.1107/S2056989025010679
Arindam Saha , Garry S Hanan , Mihaela Cibian
The title compound crystallizes with two independent molecules in the asymmetric unit, which are connected into chains by N—H⋯O hydrogen bonds.
The title compound [systematic name: N-(2,3,4,5,6-pentafluorophenyl)pyridine-4-carboxamide], C12H5F5N2O, crystallizes with two independent molecules (A and B) in the asymmetric unit in space group P1. The molecules adopt a conformation where the planes of the pentafluorophenyl and pyridyl rings have twist angles of 5.3 (1) and 14.5 (1)°. In the crystal, the molecules are connected by N—H⋯N hydrogen bonds between the amide H atom and the pyridyl nitrogen atom of an adjacent molecule to generate [110] chains of alternating A and B molecules. The packing is consolidated by C—H⋯π interactions, π–π stacking and C—H⋯O interactions and a short F⋯F contact of 2.7270 (13) Å occurs. The structures of related isonicotinamides are surveyed.
{"title":"Synthesis and structure of N-(perfluorophenyl)isonicotinamide","authors":"Arindam Saha , Garry S Hanan , Mihaela Cibian","doi":"10.1107/S2056989025010679","DOIUrl":"10.1107/S2056989025010679","url":null,"abstract":"<div><div>The title compound crystallizes with two independent molecules in the asymmetric unit, which are connected into chains by N—H⋯O hydrogen bonds.</div></div><div><div>The title compound [systematic name: <em>N</em>-(2,3,4,5,6-pentafluorophenyl)pyridine-4-carboxamide], C<sub>12</sub>H<sub>5</sub>F<sub>5</sub>N<sub>2</sub>O, crystallizes with two independent molecules (<em>A</em> and <em>B</em>) in the asymmetric unit in space group <em>P</em>1. The molecules adopt a conformation where the planes of the pentafluorophenyl and pyridyl rings have twist angles of 5.3 (1) and 14.5 (1)°. In the crystal, the molecules are connected by N—H⋯N hydrogen bonds between the amide H atom and the pyridyl nitrogen atom of an adjacent molecule to generate [110] chains of alternating <em>A</em> and <em>B</em> molecules. The packing is consolidated by C—H⋯π interactions, π–π stacking and C—H⋯O interactions and a short F⋯F contact of 2.7270 (13) Å occurs. The structures of related isonicotinamides are surveyed.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 19-23"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963257","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}
The cobalt(II) complex, [C30H22CoN8O4], crystallizes in the monoclinic space group P21/c, with the Co+2 ion adopting an octahedral coordination environment. The crystal structure features N—H⋯O hydrogen bonds and C—H⋯π contacts forming a chain along [011]. Hirshfeld surface analysis indicates that H⋯C/C⋯H and H⋯H contacts dominate the intermolecular interactions.
The title complex, [Co(C8H5N2O2)2(C7H6N2)2], crystallizes in the monoclinic space group P21/c with one-half of the molecule in the asymmetric unit. The Co2+ ion exhibits a distorted octahedral environment formed by two monodentate benzimidazole ligands and two bidentate benzimidazole-2-carboxylate ligands. The crystal packing features N—H⋯O hydrogen bonds and C—H⋯π contacts, which generate a chain along [011]. Hirshfeld surface analysis shows that H⋯C/C⋯H (36.2%) and H⋯H (35.3%) contacts dominate the intermolecular interactions, followed by O⋯H/H⋯O and N⋯H/H⋯N contributions.
{"title":"Synthesis, crystal structure and Hirshfeld surface analysis of bis(1H-benzimidazole-κN3)bis(benzimidazole-2-carboxylato-κ2N3,O)cobalt(II)","authors":"Farangiz Khujayeva , Sardor Murodov , Rukhshona Muratkulova , Soliha Rixsiboyeva , Kambarali Turgunov , Bakhodir Tashkhodjaev , Shakhlo Daminova","doi":"10.1107/S2056989025011211","DOIUrl":"10.1107/S2056989025011211","url":null,"abstract":"<div><div>The cobalt(II) complex, [C<sub>30</sub>H<sub>22</sub>CoN<sub>8</sub>O<sub>4</sub>], crystallizes in the monoclinic space group <em>P2</em><sub>1</sub><em>/c</em>, with the Co<sup>+2</sup> ion adopting an octahedral coordination environment. The crystal structure features N—H⋯O hydrogen bonds and C—H⋯π contacts forming a chain along [011]. Hirshfeld surface analysis indicates that H⋯C/C⋯H and H⋯H contacts dominate the intermolecular interactions.</div></div><div><div>The title complex, [Co(C<sub>8</sub>H<sub>5</sub>N<sub>2</sub>O<sub>2</sub>)<sub>2</sub>(C<sub>7</sub>H<sub>6</sub>N<sub>2</sub>)<sub>2</sub>], crystallizes in the monoclinic space group <em>P2</em><sub>1</sub><em>/c</em> with one-half of the molecule in the asymmetric unit. The Co<sup>2+</sup> ion exhibits a distorted octahedral environment formed by two monodentate benzimidazole ligands and two bidentate benzimidazole-2-carboxylate ligands. The crystal packing features N—H⋯O hydrogen bonds and C—H⋯π contacts, which generate a chain along [011]. Hirshfeld surface analysis shows that H⋯C/C⋯H (36.2%) and H⋯H (35.3%) contacts dominate the intermolecular interactions, followed by O⋯H/H⋯O and N⋯H/H⋯N contributions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 91-95"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963222","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}
The isotypic strontium analogue of the mineral henmilite, Sr2Cu(OH)4[B(OH)4]2, displays a quasi two-dimensional spin system with CuII ions.
Single crystals of distrontium copper(II) tetrahydroxide bis(tetrahydroxidoborate), Sr2Cu(OH)4[B(OH)4]2, were obtained by an ammonia evaporation method at room temperature. The compound crystallizes in the triclinic system, space group P1, and is isotypic with the calcium analogue henmilite, Ca2Cu(OH)4[B(OH)4]2. The {Cu(OH)4} units form a deformed square lattice in the ac plane, giving rise to a quasi-two-dimensional arrangement of CuII ions. An intricate network of O—H⋯O hydrogen bonds of medium strengths with the [B(OH)4] units as the primary donor groups consolidate the framework structure.
{"title":"Synthesis and crystal structure of Sr2Cu(OH)4[B(OH)4]2","authors":"Hibiki Kunisawa , Jun-ichi Yamaura , Toshihiro Nomura","doi":"10.1107/S2056989025011491","DOIUrl":"10.1107/S2056989025011491","url":null,"abstract":"<div><div>The isotypic strontium analogue of the mineral henmilite, Sr<sub>2</sub>Cu(OH)<sub>4</sub>[B(OH)<sub>4</sub>]<sub>2</sub>, displays a quasi two-dimensional spin system with Cu<sup>II</sup> ions.</div></div><div><div>Single crystals of distrontium copper(II) tetrahydroxide bis(tetrahydroxidoborate), Sr<sub>2</sub>Cu(OH)<sub>4</sub>[B(OH)<sub>4</sub>]<sub>2</sub>, were obtained by an ammonia evaporation method at room temperature. The compound crystallizes in the triclinic system, space group <em>P</em>1, and is isotypic with the calcium analogue henmilite, Ca<sub>2</sub>Cu(OH)<sub>4</sub>[B(OH)<sub>4</sub>]<sub>2</sub>. The {Cu(OH)<sub>4</sub>} units form a deformed square lattice in the <em>ac</em> plane, giving rise to a quasi-two-dimensional arrangement of Cu<sup>II</sup> ions. An intricate network of O—H⋯O hydrogen bonds of medium strengths with the [B(OH)<sub>4</sub>] units as the primary donor groups consolidate the framework structure.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 103-106"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963229","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}
Pub Date : 2026-01-01DOI: 10.1107/S2056989025011028
Aidan P. McKay , David B. Cordes , Mohd Abdul Fatah Abdul Manan
The crystal structures of a solvated and an unsolvated dithiocarbazate imine derivatives are compared and contrasted.
The syntheses and structures of 2-fluorobenzyl (Z)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate dimethyl sulfoxide monosolvate, C16H12FN3OS2·C2H6OS (1) and 2-fluorobenzyl (Z)-2-(5-bromo-2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate, C16H11BrFN3OS2 (2) are reported. Both structures feature a Z-configuration with respect to the C=N bond and the fluorobenzyl ring is approximately orthogonal to the isatin moiety. For 1, the crystal packing features weak Car—H⋯S (ar = aromatic) hydrogen bonds that link adjacent molecules in a C(10) fashion to form pleated chains propagating along [001] and short S⋯O contacts between dimethyl sulfoxide solvent molecules forming chains along [010]. The N—H hydrogen bond donors in 1 form either intramolecular or discrete N—H⋯O(DMSO) hydrogen bonds. In 2, alternating R22(8)-type pairwise N—H⋯O hydrogen bonds and short F⋯Br contacts link the molecules into chains propagating along [210]. The later unsolvated structure is of notably poorer quality and exhibits disorder in its o-fluorobenzyl group, with a 180° flip and a small twist around the S—C bond. These findings are consistent with the results of Hirshfeld surface analyses.
{"title":"Different intermolecular interactions in solvated and unsolvated isatin-based dithiocarbazate imine derivatives","authors":"Aidan P. McKay , David B. Cordes , Mohd Abdul Fatah Abdul Manan","doi":"10.1107/S2056989025011028","DOIUrl":"10.1107/S2056989025011028","url":null,"abstract":"<div><div>The crystal structures of a solvated and an unsolvated dithiocarbazate imine derivatives are compared and contrasted.</div></div><div><div>The syntheses and structures of 2-fluorobenzyl (<em>Z</em>)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate dimethyl sulfoxide monosolvate, C<sub>16</sub>H<sub>12</sub>FN<sub>3</sub>OS<sub>2</sub>·C<sub>2</sub>H<sub>6</sub>OS (<strong>1</strong>) and 2-fluorobenzyl (<em>Z</em>)-2-(5-bromo-2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate, C<sub>16</sub>H<sub>11</sub>BrFN<sub>3</sub>OS<sub>2</sub> (<strong>2</strong>) are reported. Both structures feature a <em>Z</em>-configuration with respect to the C=N bond and the fluorobenzyl ring is approximately orthogonal to the isatin moiety. For <strong>1</strong>, the crystal packing features weak C<sub>ar</sub>—H⋯S (ar = aromatic) hydrogen bonds that link adjacent molecules in a <em>C</em>(10) fashion to form pleated chains propagating along [001] and short S⋯O contacts between dimethyl sulfoxide solvent molecules forming chains along [010]. The N—H hydrogen bond donors in <strong>1</strong> form either intramolecular or discrete N—H⋯O<sub>(DMSO)</sub> hydrogen bonds. In <strong>2</strong>, alternating <em>R</em><sup>2</sup><sub>2</sub>(8)-type pairwise N—H⋯O hydrogen bonds and short F⋯Br contacts link the molecules into chains propagating along [210]. The later unsolvated structure is of notably poorer quality and exhibits disorder in its <em>o</em>-fluorobenzyl group, with a 180° flip and a small twist around the S—C bond. These findings are consistent with the results of Hirshfeld surface analyses.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 72-76"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963219","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}
The crystal structure of the complex tetrachloridobis(1H-imidazo[4,5-b]pyridin-4-ium-κN3)iron(II) has been determined. The compound crystallizes in the monoclinic system and shows an octahedral coordination environment around the Fe centre.
The title coordination complex tetrachloridobis(1H-imidazo[4,5-b]pyridin-4-ium-κN3)iron(II), [FeCl4(C6H6N3)2] or [FeCl4(LH)2], was synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in the triclinic space group P1. The iron atom (site symmetry
) is hexa-coordinated, adopting a slightly distorted octahedral geometry defined by two 1H-imidazo[4,5-b]pyridinium ligands and four chloride anions. In the crystal, N—H⋯Cl hydrogen bonds generate two-dimensional layers parallel to the ab plane, while the three-dimensional supramolecular framework is further consolidated by C—H⋯Cl interactions. In addition, π–π stacking interactions contribute to the overall cohesion of the crystal structure. Hirshfeld surface analysis indicates the significance of various intermolecular contacts in the crystal packing, with major contributions from Cl⋯H/H⋯Cl (43.2%), H⋯H (22.5%), C⋯H/H⋯C (16.4%), H⋯N/N⋯H (4.4%), N⋯C/C⋯N (3.7%), C⋯C (3.6%), Cl⋯N/N⋯Cl (3.2%), Cl⋯C/C⋯Cl (2.4%), and N⋯N (0.6%) interactions.
{"title":"Crystal structure and Hirshfeld surface analysis of [FeCl4(LH)2] (LH = 1H-imidazo[4,5-b]pyridin-4-ium)","authors":"Soffa Imene , Bouhidel Zakaria , Sahli Kaouther , Cherouana Aouatef , Bendeif El-Eulmi","doi":"10.1107/S2056989025010564","DOIUrl":"10.1107/S2056989025010564","url":null,"abstract":"<div><div>The crystal structure of the complex tetrachloridobis(1<em>H</em>-imidazo[4,5-<em>b</em>]pyridin-4-ium-κ<em>N</em><sup>3</sup>)iron(II) has been determined. The compound crystallizes in the monoclinic system and shows an octahedral coordination environment around the Fe centre.</div></div><div><div>The title coordination complex tetrachloridobis(1<em>H</em>-imidazo[4,5-<em>b</em>]pyridin-4-ium-κ<em>N</em><sup>3</sup>)iron(II), [FeCl<sub>4</sub>(C<sub>6</sub>H<sub>6</sub>N<sub>3</sub>)<sub>2</sub>] or [FeCl<sub>4</sub>(LH)<sub>2</sub>], was synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in the triclinic space group <em>P</em>1. The iron atom (site symmetry <blockquote><div><figure></figure></div></blockquote>) is hexa-coordinated, adopting a slightly distorted octahedral geometry defined by two 1<em>H</em>-imidazo[4,5-<em>b</em>]pyridinium ligands and four chloride anions. In the crystal, N—H⋯Cl hydrogen bonds generate two-dimensional layers parallel to the <em>ab</em> plane, while the three-dimensional supramolecular framework is further consolidated by C—H⋯Cl interactions. In addition, π–π stacking interactions contribute to the overall cohesion of the crystal structure. Hirshfeld surface analysis indicates the significance of various intermolecular contacts in the crystal packing, with major contributions from Cl⋯H/H⋯Cl (43.2%), H⋯H (22.5%), C⋯H/H⋯C (16.4%), H⋯N/N⋯H (4.4%), N⋯C/C⋯N (3.7%), C⋯C (3.6%), Cl⋯N/N⋯Cl (3.2%), Cl⋯C/C⋯Cl (2.4%), and N⋯N (0.6%) interactions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 10-13"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963291","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}
Pub Date : 2026-01-01DOI: 10.1107/S2056989025010862
Takumi Kinoshita , Hiroshi Segawa
In the title RuII complex, a meridionally bound 4,4′,4′′-tris(methoxycarbonyl)terpyridine and a dimethoxyphenylphosphine ligand define a distorted trans-RuN3PCl2 octahedral coordination environment, and water molecules of crystallization bridge pairs of complex molecules into discrete hydrogen-bonded dimers.
In the title compound, [RuCl2(C21H17N3O6)(C8H11O2P)]·H2O, the RuII atom is coordinated by three N atoms of a meridionally bound 4,4′,4′′-tris(methoxycarbonyl)-2,2′:6′,2′′-terpyridine ligand, a phosphinite P donor and two chloride ligands in a distorted octahedral geometry. The Ru—N distances lie in the range 1.996 (2)–2.078 (2) Å, with a Ru—P distance of 2.2879 (9) Å and Ru—Cl distances of 2.3713 (8) and 2.4191 (8) Å; the N—Ru—N bite angles are 78.59 (9) and 79.10 (9)°, with an N—Ru—N angle of 157.30 (9)° within the terpyridine chelate. The methyl ester groups adopt conformations that minimize steric interactions with the phosphinite phenyl ring and provide potential anchoring sites in the corresponding carboxylic acid dye. In the crystal, pairs of complex molecules are linked into discrete hydrogen-bonded dimers by the water molecule of crystallization: one H atom forms an O—H⋯O contact to a methyl carbonyl O atom [H⋯O = 2.17 Å] and the other H atom forms an O—H⋯Cl contact to a trans chloride ligand of a neighbouring complex [H⋯Cl = 2.40 Å].
{"title":"Crystal structure and near-infrared emission of trans-dichlorido(dimethoxyphenylphosphine)[4,4′,4′′-tris(methoxycarbonyl)-2,2′:6′,2′′-terpyridine]ruthenium(II) monohydrate","authors":"Takumi Kinoshita , Hiroshi Segawa","doi":"10.1107/S2056989025010862","DOIUrl":"10.1107/S2056989025010862","url":null,"abstract":"<div><div>In the title Ru<sup>II</sup> complex, a meridionally bound 4,4′,4′′-tris(methoxycarbonyl)terpyridine and a dimethoxyphenylphosphine ligand define a distorted <em>trans</em>-RuN<sub>3</sub>PCl<sub>2</sub> octahedral coordination environment, and water molecules of crystallization bridge pairs of complex molecules into discrete hydrogen-bonded dimers.</div></div><div><div>In the title compound, [RuCl<sub>2</sub>(C<sub>21</sub>H<sub>17</sub>N<sub>3</sub>O<sub>6</sub>)(C<sub>8</sub>H<sub>11</sub>O<sub>2</sub>P)]·H<sub>2</sub>O, the Ru<sup>II</sup> atom is coordinated by three N atoms of a meridionally bound 4,4′,4′′-tris(methoxycarbonyl)-2,2′:6′,2′′-terpyridine ligand, a phosphinite P donor and two chloride ligands in a distorted octahedral geometry. The Ru—N distances lie in the range 1.996 (2)–2.078 (2) Å, with a Ru—P distance of 2.2879 (9) Å and Ru—Cl distances of 2.3713 (8) and 2.4191 (8) Å; the N—Ru—N bite angles are 78.59 (9) and 79.10 (9)°, with an N—Ru—N angle of 157.30 (9)° within the terpyridine chelate. The methyl ester groups adopt conformations that minimize steric interactions with the phosphinite phenyl ring and provide potential anchoring sites in the corresponding carboxylic acid dye. In the crystal, pairs of complex molecules are linked into discrete hydrogen-bonded dimers by the water molecule of crystallization: one H atom forms an O—H⋯O contact to a methyl carbonyl O atom [H⋯O = 2.17 Å] and the other H atom forms an O—H⋯Cl contact to a <em>trans</em> chloride ligand of a neighbouring complex [H⋯Cl = 2.40 Å].</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"82 1","pages":"Pages 51-55"},"PeriodicalIF":0.6,"publicationDate":"2026-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145963228","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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