Acta Crystallographica Section C Structural Chemistry最新文献

{"title":"Salt forms of the monoazo dye Mordant Orange 1.","authors":"Alan R Kennedy, Connor MacCall, Michael W Reid, Ben Shaw, Maxwell Taylor","doi":"10.1107/S2053229626006765","DOIUrl":"10.1107/S2053229626006765","url":null,"abstract":"<p><p>The crystal structures of eight salt forms of the carboxylate-functionalized monoazo dye Mordant Orange 1 are presented and discussed, primarily in terms of their coordination behaviour. The relatively non-polar metals Mg and Li give the solvent-separated ion-pair structures hexaaquamagnesium bis{2-hydroxy-5-[(E)-(4-nitrophenyl)diazenyl]benzoate} tetrahydrate, [Mg(H₂O)₆](C₁₃H₈N₃O₅)₂·4H₂O, and tetraaqualithium 2-hydroxy-5-[(E)-(4-nitrophenyl)diazenyl]benzoate dihydrate, [Li(H₂O)₄](C₁₃H₈N₃O₅)·2H₂O, respectively. The alkaline earth metals Sr and Ba give isostructural catena-poly[[[(dimethylformamide)strontium(II)]-μ-aqua-bis{μ-2-hydroxy-5-[(E)-(4-nitrophenyl)diazenyl]benzoato}] dimethylformamide disolvate] and the barium(II) analogue, {[M(C₁₃H₈N₃O₅)₂(DMF)(H₂O)]·2DMF}_n (M = Sr, Ba; DMF is dimethylformamide, C₃H₇NO), and a crystallographic mirror plane passes through the metal centre and the DMF ligand. These are 1D coordination polymers that propagate via M-O-M bridges where the O atom is from a carboxylate group or from a water ligand. For the Na, Rb and mixed Cs/Na salt forms, namely, poly[tetra-μ-aqua-diaquabis{μ-2-hydroxy-5-[(E)-(4-nitrophenyl)diazenyl]benzoato}disodium(I)], [Na₂(C₁₃H₈N₃O₅)₂(H₂O)₆]_n, poly[tetra-μ-aqua-bis{μ-2-hydroxy-5-[(E)-(4-nitrophenyl)diazenyl]benzoato}dirubidium(I)], [Rb₂(C₁₃H₈N₃O₅)₂(H₂O)₄]_n, and poly[tetra-μ-aqua-diaquabis{μ-2-hydroxy-5-[(E)-(4-nitrophenyl)diazenyl]benzoato}caesium(I)sodium(I)], [NaCs(C₁₃H₈N₃O₅)₂(H₂O)₆]_n, the nitro substituent was found to be as competitive in its ability to bond to metal as the carboxylate group. For Na, this gave a 1D coordination polymer, where Na₄ units link through the length of the azo anions and via bonds to both nitro and carboxylate groups. For both the Rb and the mixed Cs/Na salt forms, higher metal coordination numbers and more extensive bridging interactions give 3D coordination polymers.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"427-436"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13439670/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148395580","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal and electronic structure of heteroanionic praseodymium chlorosilicate Pr₃Cl₅[SiO₄].","authors":"Ella Madura, Darren Weng, Thimira Kandabadage, Sviatoslav Baranets","doi":"10.1107/S2053229626006728","DOIUrl":"10.1107/S2053229626006728","url":null,"abstract":"<p><p>Novel heteroanionic tripraseodymium pentachloride orthosilicate, Pr₃Cl₅[SiO₄], was synthesized from a stoichiometric mixture of Pr₂O₃, PrCl₃, and SiO₂ using a self-flux-assisted high-temperature reaction under vacuum-sealed conditions. Single-crystal X-ray diffraction revealed that the compound crystallizes in the orthorhombic space group Pnma (No. 62) with unit-cell parameters a = 16.0012 (10), b = 4.1766 (2), and c = 14.0348 (9) Å (Z = 4). The structure consists of discrete [SiO₄]^4- tetrahedra within the anionic sublattice, embedded within a three-dimensional network of distorted [PrCl₇O₃] polyhedra, in which each Pr³⁺ cation is ten-coordinated in a distorted tetracapped trigonal prismatic or bicapped square-antiprismatic fashion. Refinement revealed coupled positional splitting of the Si atom and the apical O atom aligned approximately along the crystallographic b axis, corresponding to two mirror-related `up-down' orientations of the discrete [SiO₄]^4- tetrahedra in the average Pnma structure. Electronic structure calculations based on a symmetry-lowered disorder-free model generated using ISODISTORT predict an indirect bandgap of ca 4.53 eV, classifying Pr₃Cl₅[SiO₄] as a wide-bandgap insulator. The density of states (DOS) analysis indicates that the valence band is dominated by O 2p and Cl 3p states, while the conduction band is primarily derived from Pr 5d orbitals. Crystal orbital Hamilton population (COHP) and crystal orbital bond index (COBI) analyses establish a clear hierarchy of bonding strengths: Si-O (-iCOHP = 7.35 eV, iCOBI = 0.72) ≫ Pr-O (3.18 eV, 0.48) > Pr-Cl (1.62 eV, 0.27), highlighting the strongly covalent nature of Si-O bonds and weaker, but still appreciable, polar Pr-Cl and Pr-O interactions. These findings provide new insights into the crystal and electronic structure characteristics of rare-earth (RE) chlorosilicates, extending the structural chemistry of the RE₃Cl₅(SiO₄) family.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"401-406"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148395530","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":"Effect of molecular perturbation on cocrystal formation: theophylline and its 8-halo analogues with flavonoids.","authors":"Weijian Ye, Herman H Y Sung, Ian D Williams","doi":"10.1107/S2053229626006637","DOIUrl":"10.1107/S2053229626006637","url":null,"abstract":"<p><p>The tendency for cocrystal formation between alkaloids and flavonoids is found to be quite common (around 30%) and based on the optimization of hydrogen-bond formation between the acceptor-rich alkaloids and donor-rich flavonoids. Within each molecular family there is substantial variation in cocrystal tendency, leading to considerable scope for selective cocrystal precipitation to assist in the separation of complex mixtures of these natural product families. Theophylline (C₇H₈N₄O₂) follows caffeine and theacrine in forming a substantial number of flavonoid cocrystals - six in total, of which three were reported previously. By contrast, the 8-halo-substituted analogues 8-X-Tph [X = Cl (C₇H₇ClN₄O₂), Br (C₇H₇BrN₄O₂)] form cocrystals with just myricetin (C₁₅H₁₀O₈) and kaempferol (C₁₅H₁₀O₆). Weakening of the acceptor capability of the alkaloid N9 atom upon proximal halo substitution may play a role in the reduced tendency of 8-X-Tph towards cocrystal formation, since improved packing efficiency is not a key factor in the formation of these cocrystals. Most of the cocrystal phases may be conveniently prepared with good yield and purity through either liquid-assisted grinding (LAG) or microwave-assisted cocrystallization from 1-butanol.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"414-426"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13439671/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148395555","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":"Synthesis, structure and orange-light emission of a zero-dimensional antimony(III) halide with the 4,4'-(ethane-1,2-diyl)dipyridin-1-ium cation.","authors":"Ting Li, Yan Hong Li, Jia Yi Han, Yi Tong Wang, Min Le Han","doi":"10.1107/S2053229626006935","DOIUrl":"10.1107/S2053229626006935","url":null,"abstract":"<p><p>Exploring orange-light-emitting lead-free halides with high photoluminescence quantum yields (PLQYs) is a significant challenge in luminescent materials research. Herein, a zero-dimensional organic-inorganic hybrid halide, namely, 4,4'-(ethane-1,2-diyl)dipyridin-1-ium pentachloridoantimonate(III), (C₁₂H₁₄N₂)[SbCl₅] or [H₂bpa][SbCl₅], where bpa is 1,2-bis(pyridin-4-yl)ethane, was synthesized via acid solution evaporation. The compound crystallizes in the triclinic space group P1. The asymmetric unit consists of an [SbCl₅]^2- anion and two half [H₂bpa]²⁺ cations. The [SbCl₅]^2- anion and [H₂bpa]²⁺ cations are linked via intermolecular hydrogen bonds and π-π interactions to form a three-dimensional supramolecular architecture. Significantly, this halide exhibits highly efficient orange-light emission centred at 600 nm, with a PLQY of 65.57%.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"453-458"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13439667/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148519763","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":"Structural characterization of a series of alkali metal coordination polymers of gallic acid.","authors":"Ava Kreider-Mueller, James A Golen, Thomas A Morris, David R Manke","doi":"10.1107/S2053229626007096","DOIUrl":"10.1107/S2053229626007096","url":null,"abstract":"<p><p>This work aims to reveal the rich coordination chemistry of gallic acid (H₄GA), a ubiquitous plant polyphenol, toward alkali metals. To date, only three crystal structures have been reported in the literature that feature an alkali metal, namely Na, K, and Cs, in combination with a deprotonated form of gallic acid. Of those three structures, only the Cs compound, which is an alkali metal-based coordination polymer of gallic acid, features direct coordination between the deprotonated acid and the alkali metal center. This work reports the crystal structures of six new alkali metal-based coordination polymers of gallic acid, including poly[diaqua(μ-3,4,5-trihydroxybenzoato)(μ-3,4,5-trihydroxybenzoic acid)lithium], [Li(C₇H₅O₅)(C₇H₆O₅)(H₂O)₂]_n, 1, poly[diaqua-μ-aqua-(μ-3,4,5-trihydroxybenzoato)sodium], [Na(C₇H₅O₅)(H₂O)₃]_n, 2, poly[[tetraaquabis(μ-3,4,5-trihydroxybenzoato)bis(3,4,5-trihydroxybenzoic acid)disodium] tetrahydrate], {[Na₂(C₇H₅O₅)₂(C₇H₆O₅)₂(H₂O)₄]·4H₂O}_n, 3, poly[[μ-acetato-(μ-3,4,5-trihydroxybenzoic acid)potassium] monohydrate], {[K(C₇H₆O₅)(C₂H₃O₂)]·H₂O}_n, 4, poly[[μ-acetato-(μ-3,4,5-trihydroxybenzoic acid)rubidium]monohydrate], {[Rb(C₇H₆O₅)(C₂H₃O₂)]·H₂O}_n, 5, poly[diaquabis(μ-3,4,5-trihydroxybenzoato)-bis(μ-3,4,5-trihydroxybenzoic acid)dicaesium], [Cs₂(C₇H₅O₅)₂(C₇H₆O₅)₂(H₂O)₂]_n, 6. Single crystals suitable for X-ray diffraction studies were obtained from ethanolic solutions of H₄GA that were treated with a series of aqueous solutions of alkali metal acetates, MOAc (M = Li, Na, K, Rb, and Cs). Seven different molar ratios of MOAc to H₄GA (1:1, 1:2, 1:3, 1:4, 2:1, 3:1, and 4:1) were tested for each reaction combination. The dimensionality of the six coordination polymers reported varies across this series of compounds, ranging from one-dimensional chains (3) to two-dimensional sheets (1 and 2), and complex three-dimensional coordination network solids (4-6). Interestingly, the K (4) and Rb (5) compounds are isomorphous, while the sodium salt crystallizes in two forms (2 and 3).</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"468-484"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148547483","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A new Dion-Jacobson-type perovskite with an isomorphic phase transition.","authors":"Ya Xin Xu, Xin Yi Zheng, Bing Bing Yu, Shu Ting Yuan, Jing Yang Ma, Jin Bin Yuan, Li De Yu, Ji Qiang Liu","doi":"10.1107/S2053229626006790","DOIUrl":"10.1107/S2053229626006790","url":null,"abstract":"<p><p>Structural phase-transition materials have already received widespread attention due to their powerful functional features. However, for emerging Dion-Jacobson-type perovskites with strong intrinsic molecular interactions it is difficult to undergo structural phase transitions. Here, we synthesized a novel Dion-Jacobson (DJ) hybrid perovskite, (R)-3-(dimethylamino)pyrrolidinium tetrabromidoplumbate(III), (C₆H₁₆N₂)[PbBr₄] (PPB), by introducing a single chiral organic component. Experimental evidence reveals that PPB exhibits an isomorphic phase transition accompanied by a dielectric transition and a second-harmonic generation (SHG) response. This work presents a new phase-transition DJ hybrid perovskite functional material.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"448-452"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148468346","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal structure and optical properties of a two-dimensional lead(II) chloride porous metal halide semiconductor.","authors":"Ali Azmy, Ioannis Spanopoulos","doi":"10.1107/S2053229626007254","DOIUrl":"10.1107/S2053229626007254","url":null,"abstract":"<p><p>A new member of the recently developed family of porous metal halide semiconductors (PMHS) is reported. Crystals of bis(4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane) tetradecachloridopentaplumbate(II), {(C₁₈H₃₈N₂O₆)₂[Pb₅Cl₁₄]}_n or (DHS)₂Pb₅Cl₁₄ (DHS is the double-protonated [2.2.2]cryptand) were obtained via solution chemistry protocols, with concentrated HCl as the reaction solvent. Single-crystal X-ray diffraction (XRD) revealed a two-dimensional inorganic framework, crystallizing in the hexagonal space group P6₃/m with Z' = 1/6, separated and charge-balanced by double-protonated DHS organic cations. The corresponding material is isostructural with the previously reported water-stable (DHS)₂Pb₅Br₁₄ and both feature broad light emission at room temperature. The lead chloride layer is disordered and was modeled as two components with partial occupancies of 0.585 and 0.415. (DHS)₂Pb₅Cl₁₄ decomposes when placed in water, giving rise to PbCl₂ as a degradation product. We attribute the sharp difference in water stability between the bromide and chloride analogs to differences in hydration energy and halide ionic radius, which affect their affinity for water molecules through hydrogen bonding.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"407-413"},"PeriodicalIF":1.1,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148576589","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":"Can halogen atoms in coumarin derivatives affect the structure and antiproliferative activity of nickel(II) complexes?","authors":"Jakub Kurjan, Erika Samolova, Viktória Medvecová, Martin Kello, Ivan Potočňák","doi":"10.1107/S2053229626005942","DOIUrl":"10.1107/S2053229626005942","url":null,"abstract":"<p><p>A multistep procedure from 4-halogeno-2-hydroxyacetophenones, proceeding through 7-halogeno-4-hydroxychromen-2-ones and 7-halogeno-3-acetyl-4-hydroxychromen-2-ones, followed by condensation with 2-picolylamine, was used to synthesize a new series of halogenated coumarin Schiff bases, namely, (3E)-7-halogeno-3-(1-{[(pyridin-2-yl)methyl]amino}ethylidene)-2H-1-benzopyran-2,4(3H)-diones [7-XHL, X (halogen) = F, Cl and Br; C₁₇H₁₃XN₂O₃]. The ligands 7-XHL and analogous (3E)-6-halogeno-3-(1-{[(pyridin-2-yl)methyl]amino}ethylidene)-2H-1-benzopyran-2,4(3H)-dione (6-XHL) derivatives were used to prepare nine new Ni^II complexes, divided in series: [Ni(L/6-ClL/7-FL/7-ClL)(NO₃)], 1, 5, 7 and 8, [Ni₂(L)₂(H₂O)₄](NO₃)₂, 2, and [Ni₂(6-XL/7-BrL)₂(H₂O)₄](NO₃)₂, 3, 4, 6 and 9. All the complexes and ligands were characterized by IR spectroscopy and elemental analysis. Ligands 7-XHL were further characterized by NMR spectroscopy and single-crystal X-ray diffraction. Complexes 1-5, prepared in crystalline form, were also characterized by single-crystal X-ray diffraction. Detailed descriptions of the crystal structures in the solid state of the complexes and 7-XHL ligands are provided, including π-π interactions and unusual Ni...Ni interactions observed in all the complexes. All the complexes (except for 1 and 5) were screened for their in vitro antiproliferative activity against a panel of human cancer cell lines (MDA-MB-231, HCT-116, Jurkat, U87, A549, A2058, PaTu 8902 and HepG2), alongside a non-malignant colorectal cell line (CCD-18Co). The stability of these complexes in solution was proved by UV-Vis spectrophotometry for 72 h. Across the series, it was noted that introducing halogen substituents and varying their positions leads to a moderate increase in cytotoxicity compared with the non-halogenated parent ligand, and that complexes derived from 7-XHL are generally more active than their 6-XHL analogues.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"368-382"},"PeriodicalIF":1.1,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148315129","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":"Structures of nickel-, copper-, and zinc-salophen derivatives.","authors":"Derik A Seymour, Ritter V Amsbaugh, Charlotte G Colcord, Isabelle R Fejes, Lindsey C Gebhardt, Glenn P A Yap, Meaghan M Deegan","doi":"10.1107/S2053229626005450","DOIUrl":"10.1107/S2053229626005450","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Salen-type tetradentate Schiff base ligands are ubiquitous in coordination chemistry because of their straightforward synthesis, derivatization, and versatility as ligands for metals across the periodic table. The present work was motivated by our interest in expanding the library of bifunctional salophen systems, where basic sites are incorporated in the secondary coordination sphere of salophen-ligated metals. Here, we report and describe seven previously unreported structures of nickel-, copper-, and zinc-salophen derivatives, including two complexes that integrate amine bases in the ligand periphery. These are {4,4'-di-tert-butyl-2,2'-[1,2-phenylenebis(nitrilomethylidyne)]diphenolato}nickel(II) toluene 1.33-solvate, [Ni(C&lt;sub&gt;28&lt;/sub&gt;H&lt;sub&gt;30&lt;/sub&gt;N&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt;)]·1.33C&lt;sub&gt;7&lt;/sub&gt;H&lt;sub&gt;8&lt;/sub&gt; or (&lt;sup&gt;t&lt;/sup&gt;Bu-salophen)Ni·1.33C&lt;sub&gt;7&lt;/sub&gt;H&lt;sub&gt;8&lt;/sub&gt;, {4,4'-di-tert-butyl-2,2'-[1,2-phenylenebis(nitrilomethylidyne)]diphenolato}copper(II), [Cu(C&lt;sub&gt;28&lt;/sub&gt;H&lt;sub&gt;30&lt;/sub&gt;N&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt;)] or (&lt;sup&gt;t&lt;/sup&gt;Bu-salophen)Cu, aqua{4,4'-di-tert-butyl-2,2'-[1,2-phenylenebis(nitrilomethylidyne)]diphenolato}zinc(II) tetrahydrofuran monosolvate, [Zn(C&lt;sub&gt;28&lt;/sub&gt;H&lt;sub&gt;30&lt;/sub&gt;N&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt;)(H&lt;sub&gt;2&lt;/sub&gt;O)]·C&lt;sub&gt;4&lt;/sub&gt;H&lt;sub&gt;8&lt;/sub&gt;O or (&lt;sup&gt;t&lt;/sup&gt;Bu-salophen)Zn(OH&lt;sub&gt;2&lt;/sub&gt;)·THF, {4,4'-bis(trifluoromethyl)-2,2'-[1,2-phenylenebis(nitrilomethylidyne)]diphenolato}nickel(II), [Ni(C&lt;sub&gt;22&lt;/sub&gt;H&lt;sub&gt;12&lt;/sub&gt;F&lt;sub&gt;6&lt;/sub&gt;N&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt;)] or (CF&lt;sub&gt;3&lt;/sub&gt;-salophen)Ni, {4,4'-bis(trifluoromethyl)-2,2'-[1,2-phenylenebis(nitrilomethylidyne)]diphenolato}(pyridine)zinc(II), [Zn(C&lt;sub&gt;22&lt;/sub&gt;H&lt;sub&gt;12&lt;/sub&gt;F&lt;sub&gt;6&lt;/sub&gt;N&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt;)(C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;5&lt;/sub&gt;N)] or (CF&lt;sub&gt;3&lt;/sub&gt;-salophen)Zn(py), {4,4'-di-tert-butyl-6,6'-bis[(diisopropylamino)methyl]-2,2'-[1,2-phenylenebis(nitrilomethylidyne)]diphenolato}nickel(II), [Ni(C&lt;sub&gt;42&lt;/sub&gt;H&lt;sub&gt;60&lt;/sub&gt;N&lt;sub&gt;4&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt;)] or (&lt;sup&gt;t&lt;/sup&gt;Bu-salophen-N&lt;sup&gt;i&lt;/sup&gt;Pr&lt;sub&gt;2&lt;/sub&gt;)Ni, and {4,4'-di-tert-butyl-6,6'-bis[(diphenylamino)methyl]-2,2'-[(pyridine-3,4-diyl)bis(nitrilomethylidyne)]diphenolato}(pyridine)zinc(II) pyridine monosolvate, [Zn(C&lt;sub&gt;53&lt;/sub&gt;H&lt;sub&gt;51&lt;/sub&gt;NO&lt;sub&gt;2&lt;/sub&gt;)(C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;5&lt;/sub&gt;N)]·C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;5&lt;/sub&gt;N or (&lt;sup&gt;t&lt;/sup&gt;Bu-salpyr-NPh&lt;sub&gt;2&lt;/sub&gt;)Zn(py)·py. The metal centers in these compounds adopt structures consistent with what has been observed for other salen-type ligands described in the literature, with near ideal square-planar structures around nickel or copper, and a distorted square-pyramidal structure for the zinc complexes. The primary coordination sphere around these metals expands slightly across the row, as anticipated based on the increase in d-electron count from nickel to zinc. The solid-state packing of these compounds is also discussed, including the tendency for their flat extended π-systems to pack parallel to one another. Differences in packing are observed as functional group","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"336-350"},"PeriodicalIF":1.1,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13330813/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148161535","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":"Synthesis and structural characterization of rare-earth selenates: Yb₂(SeO₃)(SeO₄)₂(H₂O)₂, Yb(HSeO₃)(SeO₄), and Tm₂(SeO₄)₃(H₂O)₄·H₂O.","authors":"Chloe Jones, Jie Ling","doi":"10.1107/S2053229626005449","DOIUrl":"10.1107/S2053229626005449","url":null,"abstract":"<p><p>Three rare-earth selenates, namely, poly[diaquadi-μ-selenato-μ-selenito-diytterbium], [Yb₂(SeO₃)(SeO₄)₂(H₂O)₂]_n, poly[μ-(hydrogen selenito)-μ-selenato-ytterbium], [Yb(HSeO₃)(SeO₄)]_n, and poly[[tetraaquatri-μ-selenato-dithulium] monohydrate], {[Tm₂(SeO₄)₃(H₂O)₄]·H₂O}_n, were synthesized by hydrothermal methods. Single-crystal X-ray diffraction (SCXRD) analysis shows that all three compounds form three-dimensional framework structures constructed from interconnected LnO_x polyhedra (Ln = Yb, Tm; x = 7-8) and selenate (SeO₄^2-) and/or selenite (SeO₃^2-) groups. Their compositions were further supported by scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX), and their oxidation states were assessed by bond-valence-sum (BVS) calculations.</p>","PeriodicalId":7115,"journal":{"name":"Acta Crystallographica Section C Structural Chemistry","volume":" ","pages":"331-335"},"PeriodicalIF":1.1,"publicationDate":"2026-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148161495","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}