S. E. Tolstikov, G. V. Romanenko, E. V. Tretyakov, A. S. Bogomyakov
{"title":"Synthesis and Structure of Bispyrazolyl Nitronylnitroxide Biradicals","authors":"S. E. Tolstikov, G. V. Romanenko, E. V. Tretyakov, A. S. Bogomyakov","doi":"10.1134/S0022476625080165","DOIUrl":"10.1134/S0022476625080165","url":null,"abstract":"<p>The reaction of bisnitronylnitroxide with a diacetylene bridging group and diazomethane leads to the modification of the initial substrate while preserving its paramagnetic centers. As a result, new nitronylnitroxide biradicals containing a bispyrazolyl fragment were prepared. Molecular and crystal structures of the biradicals are determined by single crystal XRD.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 8","pages":"1708 - 1714"},"PeriodicalIF":1.4,"publicationDate":"2025-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144918478","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":"Non-Trivial Hexanuclear Copper(II) Complex Based on 4‑(1H-tetrazole-5-yl)Benzoic Acid and 1,10-Phenanthroline","authors":"E. A. Ermakova, K. S. Smirnova, E. V. Lider","doi":"10.1134/S0022476625080062","DOIUrl":"10.1134/S0022476625080062","url":null,"abstract":"<p>The structure of a non-trivial hexanuclear mixed-ligand [Cu<sub>6</sub>(phen)<sub>6</sub>(H<sub>2</sub>O)<sub>4</sub>L<sub>6</sub>]·2EtOH·10H<sub>2</sub>O copper(II) complex with 1,10-phenanthroline (phen) and a 4-(1<i>H</i>-tetrazole-5-yl)benzoic acid (L<sup>2–</sup>) anion is determined by single-crystal X-ray diffraction (XRD). The complex crystallizes in the <span>(Pbar{1})</span> space group. Its structure contains three crystallographically non-equivalent copper(II) atoms. Cu2 and Cu3 occur in a distorted square-pyramidal environment, and Cu1 has a 5 + 1 coordination environment. The doubly deprotonated 4-(1<i>H</i>-tetrazole-5-yl)benzoic acid molecule adopts several possible coordinations and acts as a terminal and a bridging ligand connecting copper(II) atoms with each other. As a result of intermolecular π⋯π interactions and hydrogen bonds, the hexanuclear fragments are packed into an interpenetrating supramolecular layered structure.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 8","pages":"1592 - 1598"},"PeriodicalIF":1.4,"publicationDate":"2025-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144918510","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}
M. A. Shmelev, Yu. K. Voronina, A. S. Chistyakov, G. A. Razgonyaeva, M. A. Kiskin, A. A. Sidorov, I. L. Eremenko
{"title":"Effect of the Crystallization Temperature and the N-donor Ligand Nature on the Crystal Structure of {EuCd} Complexes with Pentafluorobenzoic Acid Anions","authors":"M. A. Shmelev, Yu. K. Voronina, A. S. Chistyakov, G. A. Razgonyaeva, M. A. Kiskin, A. A. Sidorov, I. L. Eremenko","doi":"10.1134/S0022476625070133","DOIUrl":"10.1134/S0022476625070133","url":null,"abstract":"<p>Variation of the crystallization temperature of cadmium pentafluorobenzoate {[Cd(H<sub>2</sub>O)<sub>4</sub>(pfb)](pfb)}<sub><i>n</i></sub> (Hpfb = pentafluorobenzoic acid), europium pentafluorobenzoate [Eu<sub>2</sub>(H<sub>2</sub>O)<sub>8</sub>(pfb)<sub>6</sub>]·2H<sub>2</sub>O, and pyrazino[2,3-f][1,10]phenanthroline (pzphen) in MeCN results in the isolation of crystals: coordination polymer [Eu<sub>2</sub>(H<sub>2</sub>O)<sub>2</sub>Cd<sub>2</sub>(pzphen)<sub>2</sub>(pfb)<sub>10</sub>]<sub><i>n</i></sub> (<b>1</b>) at 25 °C and [Eu<sub>2</sub>Cd<sub>4</sub>(pzphen)<sub>4</sub>(pfb)<sub>14</sub>]<sub><i>n</i></sub>·4<i>n</i>MeCN (<b>2</b>) and [Eu<sub>2</sub>Cd<sub>2</sub>(pzphen)<sub>4</sub>(pfb)<sub>10</sub>]·10MeCN (<b>3</b>) compounds at 75 °C. When bathophenanthroline (bphen) and 2,9-dimethylbathophenanthroline (mbphen) are used as <i>N</i>-donor ligands, the crystallization temperature does not affect the compositions and structures of the compounds formed, and therefore, [Eu<sub>2</sub>Cd<sub>2</sub>(bphen)<sub>2</sub> (pfb)<sub>10</sub>]<sub><i>n</i></sub>·2<i>n</i>MeCN (<b>4</b>) and [Eu<sub>2</sub>Cd<sub>2</sub>(mbphen)<sub>2</sub>(pfb)<sub>10</sub>]·H<sub>2</sub>O (<b>5</b>) complexes are formed. The synthesized compounds are characterized by single crystal X-ray diffraction, IR spectroscopy, and the CHN analysis. The structures and crystal packings of the obtained complexes are examined in detail. The main contribution to the stabilization of crystal packings is made by π⋯π, C–H⋯F, C–F⋯π interactions.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 7","pages":"1474 - 1490"},"PeriodicalIF":1.4,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145161845","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}
Yu. V. Strelnikova, A. A. Iova, A. S. Ovsyannikov, D. R. Islamov, V. A. Burilov, P. V. Dorovatovskii, S. E. Solovieva, I. S. Antipin
{"title":"New Mixed-Valence Trinuclear {CoIII-CoII-CoIII}-Cluster Based on bis-Chelating N2O2-Donor Macrocyclic Schiff Base Supported by the Calix[4]Arene Platform: Synthesis and Structure","authors":"Yu. V. Strelnikova, A. A. Iova, A. S. Ovsyannikov, D. R. Islamov, V. A. Burilov, P. V. Dorovatovskii, S. E. Solovieva, I. S. Antipin","doi":"10.1134/S0022476625070169","DOIUrl":"10.1134/S0022476625070169","url":null,"abstract":"<p>Mixed-valence {Co<sup>III</sup>-Co<sup>II</sup>-Co<sup>III</sup>}-cluster is synthesized for the first time and characterized in the crystalline phase by single crystal X-ray diffraction, IR spectroscopy, HR-ESI mass spectroscopy, and thermogravimetric analysis. The cluster is stabilized by two molecules of bischelating N<sub>2</sub>O<sub>2</sub>-donor macrocyclic Schiff base supported by the 1,3-disubstituted calix[4]arene platform together with two μ–η<sup>1</sup>:η<sup>1</sup> acetate and two μ<sub>2</sub>-methylate bridging groups.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 7","pages":"1537 - 1550"},"PeriodicalIF":1.4,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145162032","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}
A. A. Osipov, S. A. Nayfert, A. N. Efremov, V. S. Senchurin, K. Radzhakumar, P. V. Dorovatovskiy, D. A. Zherebtsov
{"title":"Synthesis and Structure of a Metal-Organic Framework Based on Lanthanum(III) and Diacetylenedibenzoic Acid","authors":"A. A. Osipov, S. A. Nayfert, A. N. Efremov, V. S. Senchurin, K. Radzhakumar, P. V. Dorovatovskiy, D. A. Zherebtsov","doi":"10.1134/S0022476625070054","DOIUrl":"10.1134/S0022476625070054","url":null,"abstract":"<p>Metal-organic frameworks (MOFs) are a widely studied class of compounds characterized by porous structure and large surface area. MOFs are highly promising materials for practical applications as pollution sensors, selective sorbents, etc. There has been increasing recent interest in MOFs containing a long rigid linear linker that can significantly increase the size and area of MOF pores. Derivatives of diacetylenedibenzoic acid can be used as such ligands. In this work, a metal-organic framework based on diacetylenedibenzoic acid and lanthanum is prepared, its single crystals are obtained, and their structure is studied. The synthesis is performed by the solvothermal method using N,N-dimethylformamide (DMF) as a solvent. The structure of the obtained single crystal is determined by single crystal XRD. it is shown that this compound contains a 3D network with stretched (~4×31 Å) orthorhombic channels filled with water and DMF molecules. Lanthanum cations are interconnected into 1D chains by carboxylic groups. The coordination number of lanthanum is eight. Two neighboring La<sup>3+</sup> ions are connected into linear motifs by the oxygens of carboxylic groups. Each water molecule participates in the formation of hydrogen bonds or in the coordination of La<sup>3+</sup> ions or in these both interactions. Only half of the DMF molecules have hydrogen bonds; the other half fill MOF pores and form weak van der Waals contacts. Due to the presence of solvent filled pores, this MOF can have a developed surface area.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 7","pages":"1385 - 1394"},"PeriodicalIF":1.4,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145162336","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}
D. I. Konovalov, M. A. Shestopalov, A. A. Ivanov, Yu. A. Vorotnikov
{"title":"Supramolecular System: Rhenium γ-Cyclodextrin Cluster Complex - Keggin-Structure Polyoxometalate","authors":"D. I. Konovalov, M. A. Shestopalov, A. A. Ivanov, Yu. A. Vorotnikov","doi":"10.1134/S0022476625070108","DOIUrl":"10.1134/S0022476625070108","url":null,"abstract":"<p>Three-component supramolecular system NaH[{Re<sub>6</sub>S<sub>8</sub>}(H<sub>2</sub>O)<sub>6</sub>]@γ-CD@[SiW<sub>12</sub>O<sub>40</sub>]·12H<sub>2</sub>O is obtained by slow evaporation of an aqueous solution containing the [{Re<sub>6</sub>S<sub>8</sub>}(H<sub>2</sub>O)<sub>6</sub>]<sup>2+</sup> cluster complex, [SiW<sub>12</sub>O<sub>40</sub>]<sup>4–</sup> polyoxometalate (POM), and γ-cyclodextrin (γ-CD). The composition of the synthesized compound is confirmed by the elemental analysis, IR spectroscopy, and the single crystal X-ray diffraction analysis. The compound crystallizes in the orthorhombic crystal system, space group <i>P</i>2<sub>1</sub>2<sub>1</sub>2<sub>1</sub> with unit cell parameters <i>a = </i>22.7524(13) Å, <i>b = </i>23.8164(14) Å, <i>c = </i>23.9121(12) Å, <i>V = </i>12957.5(12) Å<sup>3</sup>, <i>Z</i> = 4. It is shown that the compound does not exhibit luminescent properties in the solid state. The luminescence intensity of the cluster complex in an aqueous solution decreases with increasing concentrations of both POM and POM@γ-CD, which can indicate the possible electron/energy transfer from the cluster excited state to POM or POM@γ-CD inclusion compound.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 7","pages":"1431 - 1439"},"PeriodicalIF":1.4,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145161851","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}
M. D. Taigina, M. I. Rakhmanova, T. S. Sukhikh, K. A. Vinogradova
{"title":"Synthesis, Structure, and Photoluminescent Properties of Copper(I) Complexes with N-(diphenylphosphino)-4-Phenylpyrimidineamine","authors":"M. D. Taigina, M. I. Rakhmanova, T. S. Sukhikh, K. A. Vinogradova","doi":"10.1134/S0022476625070042","DOIUrl":"10.1134/S0022476625070042","url":null,"abstract":"<p>Complexes of copper(I) iodide, bromide, and chloride with N-(diphenylphosphino)-4-phenylpyrimidineamine (L) are synthesized. The [Cu<sub>2</sub>L<sub>2</sub>I<sub>2</sub>] (<b>I</b>), [Cu<sub>2</sub>L<sub>2</sub>I<sub>2</sub>]·2.3MeCN (<b>II</b>), [Cu<sub>2</sub>L<sub>2</sub>Br<sub>2</sub>] ·1.5MeCN·0.5CH<sub>2</sub>Cl<sub>2</sub> (<b>III</b>), and CuLCl (<b>IV</b>) complexes are prepared by reactions of the corresponding copper(I) salts and L in organic solvents in the 1:1 molar ratio. It is shown by XRD that <b>II</b> and <b>III </b>have a binuclear molecular structure; the L molecule is coordinated to copper atoms in a bidentate cyclic mode via P and N1 atoms of the pyrimidine ring; the distorted tetrahedral environment of Cu atoms is supplemented by halide ions; the coordination polyhedron is CuNPI<sub>2</sub> (<b>II)</b> and CuNPBr<sub>2</sub> (<b>III</b>). The structure of <b>II</b> has two crystallographically independent molecules containing a {Cu<sub>2</sub>I<sub>2</sub>} fragment in <i>rhombus</i> and <i>butterfly</i> conformations, respectively. In the molecule of <b>II</b>, all {Cu<sub>2</sub>Br<sub>2</sub>} fragments have a planar rhombic structure. Solid-state photoluminescent properties of L and <b>I</b>, <b>III</b>, <b>IV</b> complexes are studied. The <b>I</b>, <b>III, IV</b> complexes demonstrate single-band red emission with a microsecond lifetime (λ<sub>exc</sub> = 400 nm) at 635 nm, 625 nm, and 640 nm, respectively. The L compound exhibits solid-state fluorescence with two emission bands at 400 nm and 480 nm.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 7","pages":"1369 - 1384"},"PeriodicalIF":1.4,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145161692","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}
N. A. Vorotnikova, A. S. Berezin, N. V. Kuratieva, M. A. Shestopalov, Y. A. Vorotnikov
{"title":"Sodium Salts of Octahedral Molybdenum Complexes with Acrylate and Methacrylate Ligands","authors":"N. A. Vorotnikova, A. S. Berezin, N. V. Kuratieva, M. A. Shestopalov, Y. A. Vorotnikov","doi":"10.1134/S0022476625070078","DOIUrl":"10.1134/S0022476625070078","url":null,"abstract":"<p>Two new molybdenum cluster complexes Na<sub>2</sub>[Mo<sub>6</sub>I<sub>8</sub>L<sub>6</sub>] (L = –CH<sub>2</sub>=CH–COO<sup>–</sup> (acrylate, Acr<sup>–</sup>) and –CH<sub>2</sub>=C(CH<sub>3</sub>)–COO<sup>–</sup> (methacrylate, MAcr<sup>–</sup>)) are prepared and studied. The complexes are prepared by solvothermal synthesis in methanol from Na<sub>2</sub>[Mo<sub>6</sub>I<sub>8</sub>(OMe)<sub>6</sub>] in the presence of small excess of the corresponding organic acid. As a result, XRD-quality single crystals of Na<sub>2</sub>[Mo<sub>6</sub>I<sub>8</sub>L<sub>6</sub>]·2MeOH are formed. The composition and purity of the phases are confirmed by the CHN elemental analysis, energy dispersion analysis, IR spectroscopy, and powder XRD. Photoluminescent properties of both complexes in the solid state and in a dimethylformamide solution are studied.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 7","pages":"1403 - 1411"},"PeriodicalIF":1.4,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145162339","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":"X-Ray Certification of Si, Ge, LaB6, and InSb Single Crystals","authors":"P. S. Serebrennikova, S. A. Gromilov","doi":"10.1134/S0022476625070157","DOIUrl":"10.1134/S0022476625070157","url":null,"abstract":"<p>We report an X-ray certification of a series of new X-ray standard (Si, Ge, LaB<sub>6</sub>, InSb) in the form of 20-50 µm large perfect high-purity single crystals. The unit cell parameters of the studied single crystals are measured using a Si single crystal (<i>a</i> = 5.431042 Å) as an external reference that was earlier studied on a single-crystal spectrometer using Bond′s scheme. It is shown that the relative accuracy of the obtained cubic unit cell parameters Δ<i>a</i>/<i>a</i> is at least 5·10<sup>–5</sup> provided that eccentricity was taken into account properly. The cubic unit cell parameter of the Y<sub>2</sub>O<sub>3</sub> single crystal is refined using Ge and InSb standards. </p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 7","pages":"1527 - 1536"},"PeriodicalIF":1.4,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145161847","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}
E. V. Pronina, T. S. Sukhikh, M. A. Shestopalov, A. A. Ivanov, Y. A. Vorotnikov
{"title":"Double Complex Salts [Mo6I8(DMSO)6] [PM12O40](NO3) (M = Mo, W)","authors":"E. V. Pronina, T. S. Sukhikh, M. A. Shestopalov, A. A. Ivanov, Y. A. Vorotnikov","doi":"10.1134/S0022476625070066","DOIUrl":"10.1134/S0022476625070066","url":null,"abstract":"<p>This work reports a synthesis and crystal structures of [Mo<sub>6</sub>I<sub>8</sub>(DMSO)<sub>6</sub>][P<i>M</i><sub>12</sub>O<sub>40</sub>](NO<sub>3</sub>) (<i>M</i> = Mo, W) double complex salts. The compounds are prepared by a reaction between the [Mo<sub>6</sub>I<sub>8</sub>(DMSO)<sub>6</sub>]<sup>4+</sup> cationic cluster and [P<i>M</i><sub>12</sub>O<sub>40</sub>]<sup>3–</sup> anionic polyoxometalates (POMs) in the 1:1 molar ratio. The luminescence quenching of the cluster complex in the presence of polyoxometalates is studied. It is shown that none of the compounds exhibits luminescent properties, thus indicating the possibility of electron/energy transfer from the excited state of the cluster complex to the polyoxometalate. The obtained results are an important step in the development of new functional materials based on hybrid cluster–POM systems.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 7","pages":"1395 - 1402"},"PeriodicalIF":1.4,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145161849","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}