Acta Crystallographica Section E: Crystallographic Communications最新文献

{"title":"Synthesis, crystal structure and Hirshfeld surface analysis of 5-methyl-2-[(1,3-thia­zol-2-yl)sulfan­yl]-1,3,4-thia­diazole","authors":"Ekaterina Kinshakova ,&nbsp;Batirbay Torambetov ,&nbsp;Manoj K Bharty ,&nbsp;Aziz Atashov ,&nbsp;Abdusamat Rasulov ,&nbsp;Shakhnoza Kadirova ,&nbsp;Rajesh G Gonnade","doi":"10.1107/S2056989025004980","DOIUrl":"10.1107/S2056989025004980","url":null,"abstract":"<div><div>The title compound contains two biologically active heterocyclic rings, 1,3,4-thia­diazole and 1,3-thia­zole, connected <em>via</em> a sulfur atom. The packing is consolidated by non-classical inter­molecular C—H⋯N hydrogen bonds and <em>π</em>–<em>π</em> stacking inter­actions.</div></div><div><div>The title compound, C₆H₅N₃S₃, consists of two biologically relevant heterocyclic units, suggesting potential biological activity and possible use as a ligand in metal complexation. The compound crystallizes in the monoclinic space group <em>P</em>2₁/<em>c</em> and features non-classical inter­molecular C—H⋯N hydrogen bonds, along with π–π stacking inter­actions that contribute to the crystal cohesion. Hirshfeld surface analysis highlights significant inter­molecular inter­actions including, among others, N⋯H/H⋯N, S⋯H/H⋯S, and S⋯C/C⋯S contacts.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 7","pages":"Pages 569-572"},"PeriodicalIF":0.6,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144590245","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}

{"title":"Crystal structure and Hirshfeld surface analysis of dimethyl 3-methyl-8-{[4-(tri­fluoro­meth­yl)phen­yl]sulfon­yl}-7,8-di­hydro-4H-4,6a-ep­oxy­benzo[b]naphtho­[1,8-de]azepine-5,6-di­carboxyl­ate","authors":"Gleb M. Burkin ,&nbsp;Selbi Annadurdyyeva ,&nbsp;Alexandra G. Kutasevich ,&nbsp;Narmina A. Guliyeva ,&nbsp;Khudayar I. Hasanov ,&nbsp;Mehmet Akkurt ,&nbsp;Gizachew Mulugeta Manahelohe","doi":"10.1107/S2056989025004426","DOIUrl":"10.1107/S2056989025004426","url":null,"abstract":"<div><div>In the crystal, mol­ecules are linked by C—H⋯O inter­actions and C—H⋯F inter­actions to form sheets parallel to the (002) plane. In addition, S—O⋯π and π–π inter­actions link mol­ecules along the <em>a-</em>axis direction. van der Waals inter­actions between mol­ecular sheets consolidate the packing.</div></div><div><div>The mol­ecular conformation of the title compound, C₂₉H₂₂F₃NO₇S, is stable due to the intra­molecular C—H⋯O hydrogen bonds. The central seven-membered ring adopts a distorted chair form. In the 7-oxabi­cyclo­[2.2.1]hepta-2,5-diene unit, the five-membered rings adopt envelope conformations. In the crystal, the mol­ecules are linked by C—H⋯O and C—H⋯F inter­actions, forming sheets parallel to the (002) plane. Additionally, S—O⋯π and π–π inter­actions [centroid-to-centroid distance = 3.6159 (7) Å] connect the mol­ecules along the <em>a-</em>axis direction. van der Waals inter­actions between the mol­ecular sheets reinforce the mol­ecular packing. A Hirshfeld surface analysis was conducted to visualize the various inter­molecular inter­actions, indicating that the largest contribution to the surface contacts is from H⋯H inter­actions (37.3%), followed by O⋯H/H⋯O (24.1%), F⋯H/H⋯F (19.0%), and C⋯H/H⋯C (10.3%) inter­actions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 543-548"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245697","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}

{"title":"Crystal structure and characterization of a new chain-like polyrotaxane zinc(II) coordination polymer with mixed pyridine-2,6-di­carboxyl­ate and 1,4-bis­(1H-imidazol-1-ylmeth­yl)benzene ligands","authors":"Chanikarn Kummuang ,&nbsp;Kittipong Chainok ,&nbsp;Nanthawat Wannarit","doi":"10.1107/S2056989025004608","DOIUrl":"10.1107/S2056989025004608","url":null,"abstract":"<div><div>The crystal structure of a new polyrotaxane Zn^II coordination polymer, {[Zn₂(2,6-PDC)₂(bix)₂]·9H₂O}_<em>n</em>, is comprised of dinuclear macrocyclic units and a zigzag chain-like structure extending parallel to [101].</div></div><div><div>A new chain-like polyrotaxane Zn^II coordination polymer, <em>catena</em>-poly[[[[(pyridine-2,6-di­carboxyl­ato-κ³<em>O</em>,<em>N</em>,<em>O</em>′)zinc(II)]-μ-1,4-bis­(1<em>H</em>-imidazol-1-ylmeth­yl)benzene-κ²<em>N</em>¹:<em>N</em>^1′] hemi{bis­[μ-1,4-bis­(1<em>H</em>-imidazol-1-ylmeth­yl)benzene-κ²<em>N</em>¹:<em>N</em>^1′]bis­[(pyridine-2,6-di­carboxyl­ato-κ³<em>O</em>,<em>N</em>,<em>O</em>′)zinc(II)]}] nona­hydrate], {[Zn(C₇H₃NO₄)(C₁₄H₁₄N₄)][Zn₂(C₇H₃NO₄)₂(C₁₄H₁₄N₄)₂]_0.5·9H₂O}_<em>n</em> or {[Zn₂(2,6-PDC)₂(bix)₂]·9H₂O}_<em>n</em> [where 2,6-PDC = pyridine-2,6-di­carboxyl­ate, C₇H₃NO₄, and bix = 1,4-bis­(1<em>H</em>-imidazol-1-ylmeth­yl)benzene, C₁₄H₁₄N₄], was synthesized and characterized. The mol­ecular structure comprises two Zn^II units. Both Zn^II ions are fivefold coordinated, with the coordination sphere inter­mediate between trigonal-bipyramidal and square-pyramidal, as defined by two bix ligands and one 2,6-PDC tridentate chelating ligand. For one of the units, two Zn^II ions are bridged by <em>gauche</em>-bix ligands, providing a dinuclear [Zn₂(2,6-PDC)₂(bix)₂] macrocycle. The other unit is built by <em>trans</em>-bix bridging ligands, leading to a zigzag chain-like structure. Inter­estingly, these two entities are inter­weaved, leading to a polyrotaxane structure extending parallel to [101]. The crystal structure is consolidated by hydrogen-bonding, π–π and C—H⋯π inter­molecular inter­actions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 559-564"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245695","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}

{"title":"Reversible phase transition in 8,19-dimethyl-2,3,8,19-tetra­aza­penta­cyclo[13.7.0.04,12.06,10.017,21]docosa-1(15),2,4(12),5,10,16,21-hepta­ene-7,9,18,20-tetrone","authors":"Christian Näther ,&nbsp;Artjom Businski ,&nbsp;Rainer Herges","doi":"10.1107/S2056989025003998","DOIUrl":"10.1107/S2056989025003998","url":null,"abstract":"<div><div>The title compound undergoes a reversible phase transition upon cooling, during which the space group changes from <em>P</em>2₁/<em>c</em> to <em>P</em>1, which is accompanied by a discontinuous change in the unit-cell volume. In the low-temperature phase, twinning is observed, which vanishes upon reheating to room temperature.</div></div><div><div>The crystal structure of the title compound, C₂₀H₁₄N₄O₄, was previously reported at 220 K [Businski <em>et al.</em> (2025<span><span>#</span></span>). <em>Chem. Eur. J.</em> A<strong>71</strong>, 3–8], where it crystallizes in the monoclinic space group <em>P</em>2₁/<em>c</em> with one crystallographically independent mol­ecule in a general position. In this structure, disorder of the methyl H atoms is observed. However, upon cooling a continuous splitting of the reflections occurs, that might indicate a phase transition. Therefore, data sets were measured between room temperature and 90 K upon cooling and reheating, which shows that a discontinuity in the unit-cell volume occurs between 170 and 180 K. This process is accompanied by the formation of an additional crystal domain. Both domains can be indexed separately, leading to a unit cell similar to that observed at room temperature, but with both α and β angles revealing significant deviations from 90°. Twin refinements clearly show that the structure becomes triclinic (space group <em>P</em>1) upon cooling, resulting in two crystallographically independent mol­ecules in the unit cell, for which some structural changes especially in the conformation and arrangement of the mol­ecules are observed. In the low-temperature structure, disordering of the methyl H atoms is still observed. If the crystal is reheated, the reflections of the second domain disappear and the structure can be successfully refined again in the monoclinic space group <em>P</em>2₁/<em>c</em>, indicating reversibility of the transition.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 476-481"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245704","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}

{"title":"Ortho­rhom­bic cerium(III) carbonate hydroxide studied by synchrotron powder X-ray diffraction","authors":"Liam A. V. Nagle-Cocco ,&nbsp;Robert T. Bell ,&nbsp;Nicholas A. Strange","doi":"10.1107/S2056989025003512","DOIUrl":"10.1107/S2056989025003512","url":null,"abstract":"<div><div>A synchrotron powder X-ray diffraction study of commercially obtained ‘cerium(III) carbonate hydrate’ indicates that multiple Ce-containing phases coexist, none of which are Ce₂(CO₃)₃. The majority phase is an ortho­rhom­bic phase of composition CeCO₃OH.</div></div><div><div>Cerium(III) carbonate is a precursor material for the synthesis of various Ce-containing compounds. In this work, a synchrotron powder X-ray diffraction study of commercially obtained ‘cerium(III) carbonate hydrate’ indicates that multiple Ce-containing phases are present. The majority phase CeCO₃OH (52.49%_wt) was refined using an ortho­rhom­bic <em>Pmcn</em> structure model with <em>a</em> = 5.01019 (2) Å, <em>b</em> = 8.55011 (4) Å and <em>c</em> = 7.31940 (4) Å, which is based on a reported structure for the lanthanoid carbonate mineral ancylite. Additionally, a substantial portion of the precursor material is cubic cerium(IV) oxide (47.12%_wt).</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 530-533"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245702","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}

{"title":"Some thio­ether-ketones and their related derivatives","authors":"Molly A. O’Connor ,&nbsp;Anna V. Pavlishchuk ,&nbsp;Raymond J. Butcher ,&nbsp;Vitaly V. Pavlishchuk ,&nbsp;Anthony W. Addison","doi":"10.1107/S2056989025004037","DOIUrl":"10.1107/S2056989025004037","url":null,"abstract":"<div><div>Structures are reported for two thio­ether-ketones, and for some derived hydrazones, and instances of conformational enanti­omerism are delineated. Various types of hydrogen bonds, such as weak C—H⋯S and stronger N—H⋯N and N—H⋯S hydrogen bridges are noted, and inter­molecular cases examined <em>via</em> DFT calculations.</div></div><div><div>Structural characteristics are reported for two thio­ether–ketones, <em><strong>Dtdpe</strong></em> and <em><strong>Mtdp</strong></em> [2-({2-[(2-oxo-2-phenyl­eth­yl)sulfan­yl]eth­yl}sulfan­yl)-1-phenyl­ethan-1-one, C₁₈H₁₈O₂S₂, and 2-[(2-oxo-2-phenyl­eth­yl)sulfan­yl]-1-phenyl­ethan-1-one, C₁₆H₁₄O₂S], and for related derivatives, the bis­(pyridyl­hydrazones) <em><strong>Dhpk</strong></em> and <em><strong>Prpsb</strong></em> [2-((2<em>E</em>)-2-{(2<em>Z</em>)-2-phenyl-2-[2-(pyridin-2-yl)hydrazin-1-yl­idene]ethyl­idene}hydrazin-1-yl)pyridine, C₁₈H₁₆N₆, and 2-[(2<em>Z</em>,12<em>Z</em>)-3,12-diphenyl-14-(pyridin-2-yl)-5,10-di­thia-1,2,13,14-tetra­aza­tetra­deca-2,12-dien-1-yl]pyridine, C₃₀H₃₂N₆S₂], as well as for the macrocyclic thio­carbohydrazide derivative <em><strong>Ctrsp</strong></em>[(3<em>E</em>,8<em>Z</em>)-3,9-dimethyl-1,11-di­thia-4,5,7,8-tetra­aza­cyclo­tetra­deca-3,8-diene-6-thione, C₁₀H₁₈N₄S₃]. Three of the five compounds exhibit conformational enanti­omerism in the solid state. The occurrence of intra- and inter­molecular hydrogen bonding is commented upon through quantum mechanical (DFT) calculations. Weak C—H⋯S inter­actions are noted, while stronger N—H⋯N and N—H⋯S hydrogen bridges are delineated.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 520-529"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245705","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}

{"title":"Synthesis and structural characterization of the dichloride complex formed by carb­oxy-functionalized Cu(di­aza­cyclam)2+ cation and its heterometallic coordination polymer with CdCl2","authors":"Liudmyla V. Tsymbal ,&nbsp;Irina L. Andriichuk ,&nbsp;Alexandru-Constantin Stoica ,&nbsp;Yaroslaw D. Lampeka","doi":"10.1107/S2056989025003792","DOIUrl":"10.1107/S2056989025003792","url":null,"abstract":"&lt;div&gt;&lt;div&gt;The coordination polyhedra of the Cu&lt;sup&gt;II&lt;/sup&gt; ions in mol­ecular complex &lt;strong&gt;I&lt;/strong&gt; and coordination polymer &lt;strong&gt;II&lt;/strong&gt; represent tetra­gonally elongated &lt;em&gt;trans&lt;/em&gt;-CuN&lt;sub&gt;4&lt;/sub&gt;Cl&lt;sub&gt;2&lt;/sub&gt; and &lt;em&gt;trans&lt;/em&gt;-CuN&lt;sub&gt;4&lt;/sub&gt;(H&lt;sub&gt;2&lt;/sub&gt;O)Cl octa­hedra, respectively, with the four N atoms of the macrocyclic ligand forming the equatorial plane and monodentate ligands occupying the axial positions. The coordination polyhedron of the Cd&lt;sup&gt;II&lt;/sup&gt; ion in &lt;strong&gt;II&lt;/strong&gt; is a CdO&lt;sub&gt;4&lt;/sub&gt;Cl&lt;sub&gt;2&lt;/sub&gt; distorted octa­hedron formed by two bidentately coordinated deprotonated carb­oxy­lic groups of different Cu&lt;sup&gt;II&lt;/sup&gt; macrocyclic cations and two chloride anions, one of which displays a bridging function.&lt;/div&gt;&lt;/div&gt;&lt;div&gt;&lt;div&gt;The asymmetric unit of the complex [3,10-bis­(3-carb­oxy­prop­yl)-1,3,5,8,10,12-hexa­aza­cyclo­tetra­decane-κ&lt;sup&gt;4&lt;/sup&gt;&lt;em&gt;N&lt;/em&gt;&lt;sup&gt;1&lt;/sup&gt;,&lt;em&gt;N&lt;/em&gt;&lt;sup&gt;5&lt;/sup&gt;,&lt;em&gt;N&lt;/em&gt;&lt;sup&gt;8&lt;/sup&gt;,&lt;em&gt;N&lt;/em&gt;&lt;sup&gt;12&lt;/sup&gt;]di­chlorido­copper(II), [CuCl&lt;sub&gt;2&lt;/sub&gt;(C&lt;sub&gt;16&lt;/sub&gt;H&lt;sub&gt;34&lt;/sub&gt;N&lt;sub&gt;6&lt;/sub&gt;O&lt;sub&gt;4&lt;/sub&gt;)] or [Cu(H&lt;sub&gt;2&lt;/sub&gt;&lt;em&gt;L&lt;/em&gt;)Cl&lt;sub&gt;2&lt;/sub&gt;] (&lt;strong&gt;I&lt;/strong&gt;), consists of a centrosymmetric macrocyclic Cu&lt;sup&gt;II&lt;/sup&gt; dication and a chloride anion. The components of the heterometallic compound poly[[aqua­[μ&lt;sub&gt;3&lt;/sub&gt;-3,10-bis­(3-carb­oxy­prop­yl)-1,3,5,8,10,12-hexa­aza­cyclo­tetra­dec­ane-κ&lt;sup&gt;4&lt;/sup&gt;&lt;em&gt;N&lt;/em&gt;&lt;sup&gt;1&lt;/sup&gt;,&lt;em&gt;N&lt;/em&gt;&lt;sup&gt;5&lt;/sup&gt;,&lt;em&gt;N&lt;/em&gt;&lt;sup&gt;8&lt;/sup&gt;,&lt;em&gt;N&lt;/em&gt;&lt;sup&gt;12&lt;/sup&gt;:κ&lt;sup&gt;2&lt;/sup&gt;&lt;em&gt;O&lt;/em&gt;,&lt;em&gt;O&lt;/em&gt;′:κ&lt;sup&gt;2&lt;/sup&gt;&lt;em&gt;O&lt;/em&gt;′′,&lt;em&gt;O&lt;/em&gt;′′′]-μ-chlorido-­copper(II)cadmium(II] 1.25-hydrate], {[CuCd(C&lt;sub&gt;16&lt;/sub&gt;H&lt;sub&gt;32&lt;/sub&gt;N&lt;sub&gt;6&lt;/sub&gt;O&lt;sub&gt;4&lt;/sub&gt;)Cl&lt;sub&gt;2&lt;/sub&gt;(H&lt;sub&gt;2&lt;/sub&gt;O)]·1.25H&lt;sub&gt;2&lt;/sub&gt;O}&lt;sub&gt;&lt;em&gt;n&lt;/em&gt;&lt;/sub&gt; or {[CuCd(&lt;em&gt;L&lt;/em&gt;)(H&lt;sub&gt;2&lt;/sub&gt;O)Cl&lt;sub&gt;2&lt;/sub&gt;]·1.25H&lt;sub&gt;2&lt;/sub&gt;O}&lt;sub&gt;&lt;em&gt;n&lt;/em&gt;&lt;/sub&gt; (&lt;strong&gt;II&lt;/strong&gt;) are [Cu(&lt;em&gt;L&lt;/em&gt;)(H&lt;sub&gt;2&lt;/sub&gt;O)] moieties coordinated to CdCl&lt;sub&gt;2&lt;/sub&gt; units &lt;em&gt;via&lt;/em&gt; the deprotonated carb­oxy­lic groups of the macrocycle, and four water mol­ecules of crystallization with partial occupancies. In each compound, the Cu&lt;sup&gt;II&lt;/sup&gt; ion coord­inates in the equatorial plane by the four secondary N atoms of the macrocyclic ligand, which adopts the most energetically stable &lt;em&gt;trans&lt;/em&gt;-III conformation, and two mutually &lt;em&gt;trans&lt;/em&gt; axial ligands in tetra­gonally elongated &lt;em&gt;trans&lt;/em&gt;-CuN&lt;sub&gt;4&lt;/sub&gt;Cl&lt;sub&gt;2&lt;/sub&gt; and &lt;em&gt;trans&lt;/em&gt;-CuN&lt;sub&gt;4&lt;/sub&gt;(H&lt;sub&gt;2&lt;/sub&gt;O)Cl octa­hedral geometries in &lt;strong&gt;I&lt;/strong&gt; and &lt;strong&gt;II&lt;/strong&gt;, respectively. The coordination environment of the Cd&lt;sup&gt;II&lt;/sup&gt; ion in &lt;strong&gt;II&lt;/strong&gt; is a CdO&lt;sub&gt;4&lt;/sub&gt;Cl&lt;sub&gt;2&lt;/sub&gt; distorted octa­hedron formed by two bidentately coordinated deprotonated carb­oxy­lic groups of different macrocycles and two chloride anions, one of which displays a μ&lt;sub&gt;2&lt;/sub&gt;-bridging function between the Cu&lt;sup&gt;II&lt;/sup&gt; and Cd&lt;sup&gt;II&lt;/sup&gt; ions. The extended structures of both complexes are distinctly l","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 458-463"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245708","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}

{"title":"Synthesis and structure of 1′,4′-diphenyl-1a,1′,4′,4′′,5′′,9b-hexa­hydro-2′′H-di­spiro­[cyclopropa[l]phenanthrene-1,2′-[1,4]ep­oxy­naphthalene-3′,3′′-thio­phene]","authors":"Yuewei Wen ,&nbsp;Dasan M. Thamattoor","doi":"10.1107/S2056989025004104","DOIUrl":"10.1107/S2056989025004104","url":null,"abstract":"<div><div>The title compound was inadvertently prepared as a Diels–Alder adduct between 1,3-di­phenyl­isobenzo­furan and 3-(1a,9 b-di­hydro-1<em>H</em>-cyclo­propa[<em>l</em>]phenanthren-1-yl­idene)tetra­hydro­thio­phene. A combination of fused, bridged, and spiro­cyclic ring systems are all featured within a single mol­ecular structure of this highly crowded polycyclic compound.</div></div><div><div>The title compound, C₃₉H₃₀OS, was inadvertently prepared as a Diels–Alder adduct between 1,3-di­phenyl­isobenzo­furan and 3-(1a,9b-di­hydro-1<em>H</em>-cyclo­propa[<em>l</em>]phenanthren-1-yl­idene)tetra­hydro­thio­phene. A combination of fused, bridged, and spiro­cyclic ring systems are all featured within a single mol­ecular structure of this highly crowded polycyclic compound.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 501-504"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245710","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}

{"title":"Bis(μ-thio­semicarbazide-κ3N1,S:S;κ3S:N1,S)bis­[(di­methyl­formamide-κO)(thio­semicarbazide-κ2N1,S)cadmium(II)] tetra­kis­(2,4,6-tri­nitro­phen­olate): synthesis, crystal structure and Hirshfeld surface analysis","authors":"R. Santhakumari ,&nbsp;K. Ramamurthi ,&nbsp;Manpreet Kaur ,&nbsp;Jerry P. Jasinski ,&nbsp;Suresh Sagadevan ,&nbsp;Helen Stoeckli-Evans","doi":"10.1107/S2056989025003974","DOIUrl":"10.1107/S2056989025003974","url":null,"abstract":"<div><div>The complete binuclear cation of the title complex salt is generated by a crystallographic center of symmetry and features bridging S atoms.</div></div><div><div>In the title complex salt, [Cd₂(C₃H₇NO)₂(CH₅N₃S)₄](C₆H₂N₃O₇)₄, (<strong>I</strong>), the binuclear cation is located about a crystallographic center of symmetry. The asymmetric unit of the complex cation is composed of two bidentate thio­semicarbazide ligands and one mol­ecule of di­methyl­formamide coordinated to a cadmium(II) atom. The S atom of one of the thio­semicarbazide ligands bridges the cadmium atoms about the inversion center. The positive charge of the complex is balanced by picrate anions. In the crystal, the cation is linked to the picrate anions by side-by-side bifurcated N—H⋯(O,O) hydrogen bonds in which the central O atom acts as a double acceptor for two such bonds, enclosing <em>R</em>¹₂(6) and <em>R</em>²₁(6) ring motifs. In the crystal, further N—H⋯O hydrogen bonds link the various units to form slabs lying parallel to the (001) plane and the slabs are linked by C—H⋯O hydrogen bonds, thereby forming a three-dimensional network.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 505-509"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245692","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}

{"title":"Crystal structure, computational study, and Hirshfeld analysis of exo-1,2,3,5-tetra­phenyl-1a’,9b’-di­hydro­spiro­[bi­cyclo­[3.1.0]hexane-6,1′-cyclo­propa[l]phenanthren]-2-en-4-one","authors":"Alexander D. Roth ,&nbsp;Dasan M. Thamattoor","doi":"10.1107/S2056989025004414","DOIUrl":"10.1107/S2056989025004414","url":null,"abstract":"<div><div>The reaction of dibenzonorcarynyliden(e/oid) with phencyclone was recently reported to give a congested spiro­pentane with <em>endo</em> stereochemistry. Herein it is reported that, in sharp contrast, an analogous reaction using tetra­cyclone, instead of phencyclone, gives the highly crowded title spiro­pentane but with <em>exo</em> stereochemistry as determined by X-ray crystallography.</div></div><div><div>The reaction of dibenzonorcarynyliden(e/oid) with phencyclone was recently reported to give a congested spiro­pentane with <em>endo</em> stereochemistry. Herein we report that, in sharp contrast, an analogous reaction using tetra­cyclone, instead of phencyclone, gives the highly crowded title spiro­pentane but with <em>exo</em> stereochemistry as determined by X-ray crystallography. This new tetra­cyclone adduct (C₄₄H₃₀O) crystallizes upon slow evaporation from hexa­nes/ethyl acetate in the monoclinic crystal system and <em>P</em>2₁/<em>n</em> (No. 14) space group. It has one mol­ecule in the asymmetric unit and four mol­ecules per unit cell. DLPNO-CCSD(T)/def2-TZVP//B3LYP/def2-SVP calculations indicate that the <em>endo</em> spiro­pentane diastereomers from phencyclone and tetra­cyclone are both more stable than the corresponding <em>exo</em> forms by 6.68 and 5.35 kcal mol⁻¹, respectively. As noted previously in the phencyclone system, favorable π-stacking inter­actions between the two flat biphenyl moieties in the product and transition state may lead to the preferential formation of the <em>endo</em> diastereomer. However, the ability of the phenyl rings in the 3,4-position of the tetra­cyclone component to rotate could introduce destabilizing steric inter­actions in the transition state that hinder formation of the <em>endo</em> diastereomer in favor of the less thermodynamically stable <em>exo</em> isomer.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"81 6","pages":"Pages 554-558"},"PeriodicalIF":0.5,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144245700","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}