{"title":"LBO Crystallization in the Li2O–B2O3–LiF System","authors":"E. V. Khan, K. A. Kokh","doi":"10.1134/S0022476625090124","DOIUrl":"10.1134/S0022476625090124","url":null,"abstract":"<p>Phase equilibria in the Li<sub>2</sub>O–B<sub>2</sub>O<sub>3</sub>–LiF ternary system are studied. It is established that the LBO primary crystallization region has a narrow concentration interval limited by Li<sub>3</sub>B<sub>7</sub>O<sub>12</sub>–LiF and Li<sub>2</sub>B<sub>8</sub>O<sub>18</sub>–LiF lines. The hydropyrolysis of LiF in air is studied. It is shown experimentally that the decomposition of LiF from the LiBO<sub>2</sub>–LiF melt at 800 °C is insignificant, but the LiF content decreases notably with time at 900 °C.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1903 - 1907"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248295","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. S. Kolevatov, N. O. Druzhkov, I. A. Yakushev, P. V. Dorovatovskii, A. V. Piskunov
{"title":"Metal-Organic Frameworks of Zinc with Tetrazine and Carboxylate Ligands","authors":"D. S. Kolevatov, N. O. Druzhkov, I. A. Yakushev, P. V. Dorovatovskii, A. V. Piskunov","doi":"10.1134/S0022476625090203","DOIUrl":"10.1134/S0022476625090203","url":null,"abstract":"<p>The reaction of zinc nitrate with 3,6-di-4-pyridyl-1,2,4,5-tetrazine (4-DPT), 3,6-di-3-pyridyl-1,2,4,5-tetrazine (3-DPT), and <i>trans</i>-β-hydromuconic acid (H<sub>2</sub>TBHMA) yields new MOFs of the following compositions: [Zn(3-DPT)(DMF)(NO<sub>3</sub>)<sub>2</sub>] (<b>1</b>), [Zn(3-DPT)(TBHMA)]·(MeOH) (<b>2</b>·MeOH), and [Zn<sub>2</sub>(4-DPT)<sub>2</sub>(TBHMA)(NO<sub>3</sub>)<sub>2</sub>]·2MeOH (<b>3</b>·2MeOH). Structures of the compounds are studied by single crystal X-ray diffraction (CIF file CCDC Nos. 2450436(<b>1</b>), 2450437 (<b>2</b>), 2450438 (<b>3</b>)).</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1985 - 1996"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248306","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}
L. V. Frantsuzova, D. P. Gerasimova, I. R. Gilfanov, L. E. Nikitina, D. V. Zakharychev, O. A. Lodochnikova
{"title":"Polymorphism with a Varying Type of Stereoisomeric Recognition: Two Crystal Modifications of Isobornylacetamide","authors":"L. V. Frantsuzova, D. P. Gerasimova, I. R. Gilfanov, L. E. Nikitina, D. V. Zakharychev, O. A. Lodochnikova","doi":"10.1134/S0022476625090215","DOIUrl":"10.1134/S0022476625090215","url":null,"abstract":"<p>Two known polymorphic modifications of racemic isobornylacetamide (<i>C</i>2/<i>c</i> (<b>1a</b>) and <i>P</i>2<sub>1</sub>/<i>n</i> (<b>1b</b>) space groups) are prepared quantitatively for the first time and are characterized in comparison with each other using physico-chemical methods such as low-temperature XRD, DSC, and IR spectroscopy. The alternation of molecules of opposite configurations in the H-bonded chain of the crystal of <b>1b</b> leads to the formation of stronger hydrogen bonding than in the homo-chiral chain of the crystal of <b>1a</b> (as is indicated by the XRD and IR spectroscopy data on the H-bond parameters) and a larger number of secondary interactions. Thermochemical parameters of both modifications are obtained for the first time by DSC, and it is shown that the <b>1b</b> polymorph is thermodynamically preferable in the melting point region.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1997 - 2006"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248305","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. S. Popova, A. D. Maximova, D. R. Chernyavskiy, N. V. Cherkashina, M. V. Panina, O. V. Sulimova, E. A. Sosunov, P. V. Dorovatovskii, M. N. Vargaftik, I. A. Yakushev
{"title":"Hidden Complexity of a Simple Compound: Unexpected Polymorphism of Tetranuclear Platinum (II) Acetate Pt4(OCOMe)8","authors":"A. S. Popova, A. D. Maximova, D. R. Chernyavskiy, N. V. Cherkashina, M. V. Panina, O. V. Sulimova, E. A. Sosunov, P. V. Dorovatovskii, M. N. Vargaftik, I. A. Yakushev","doi":"10.1134/S0022476625090148","DOIUrl":"10.1134/S0022476625090148","url":null,"abstract":"<p>Polymorphism is an infrequent phenomenon in platinum group complexes. Surprisingly, we found a new monoclinic crystal modification (<i>C</i>2/<i>c</i>) of a relatively simple compound, platinum (II) acetate Pt<sub>4</sub>(OCOMe)<sub>8</sub> (<b>2</b>) (monoclinic <i>C</i>2/<i>c</i> (<b>2</b>), monoclinic <i>P</i>2<sub>1</sub>/<i>c</i> (<b>3</b>) and tetragonal <i>P</i>4<sub>3</sub>2<sub>1</sub>2 (<b>4</b>)). The polymorph was prepared by a novel synthetic protocol and structurally identified by single-crystal X-ray diffraction (SC-XRD) using synchrotron radiation X-ray source. Examination of the intermolecular interaction by Hirshfeld surface analysis of <b>2</b> and its comparison with another known polymorphs - monoclinic (<i>P</i>2<sub>1</sub>/<i>c</i>, <b>3</b>) and tetragonal (<i>P</i>4<sub>3</sub>2<sub>1</sub>2, <b>4</b>) ones, - as well as analysis of packaging motifs revealed the responsibility of weak interactions for their formation.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1922 - 1931"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248385","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":"Structure-Forming Complexes in Solutions: 3,5-Dimethylpyrazole–Trifluoroacetic Acid –N,N-Dimethylformamide","authors":"E. G. Tarakanova, V. D. Maiorov, I. S. Kislina","doi":"10.1134/S0022476625090082","DOIUrl":"10.1134/S0022476625090082","url":null,"abstract":"<p>IR spectroscopy and quantum chemical methods are applied to study the compositions, structures, and energy parameters of acid-basic complexes formed in three-component solutions of 3,5-dimethylpyrazole (DMP)–trifluoroacetic acid (TFAA)–N,N-dimethylformamide (DMF) at DMP:TFAA molar ratios of 1:1 and 1:2. The DMP·TFAA·DMF trimer is found to be the structure-forming fragment in the 1:1:1 solution, and in 1:1:≥2 solutions, it is the DMP·TFAA·2DMF tetramer. Both complexes have the cyclic structures and contain quasi-ionic pairs in which protons of TFAA molecules move away from them but do not transfer to DMP molecules. Cyclic tetramer DMP·2TFAA·DMF with alternating acid and base molecules is the structure-forming fragment in the DMP–TFAA–DMF triple system with DMP:TFAA = 1:2 in the entire concentration range. It consists of two quasi-ionic pairs with O⋯H⋯O and N⋯H⋯O hydrogen bridges (the TFAA molecule proton passes to the DMP molecule in it). The obtained results can be used to predict the catalytic activity of multicomponent acid solutions.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1864 - 1872"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248246","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}
S. A. Naifert, A. A. Osipov, V. S. Senchurin, M. V. Borisov, G. V. Klyukin, K. Radjakumar, D. V. Spiridonova, D. A. Zherebtsov
{"title":"Synthesis and Structure of 4-Acetyl-N,N,N-Trimethylanilinium Iodide","authors":"S. A. Naifert, A. A. Osipov, V. S. Senchurin, M. V. Borisov, G. V. Klyukin, K. Radjakumar, D. V. Spiridonova, D. A. Zherebtsov","doi":"10.1134/S0022476625090197","DOIUrl":"10.1134/S0022476625090197","url":null,"abstract":"<p>4-Acetyl-<i>N</i>,<i>N</i>,<i>N</i>-trimethylanilinium iodide (<b>1</b>) is obtained by the <i>N</i>-alkylation reaction of 4-((trimethylsilyl) ethynyl)aniline. The structure of compound <b>1</b> is solved using the single crystal X-ray diffraction analysis for the first time. 4-Acetyl-<i>N</i>,<i>N</i>,<i>N</i>-trimethylanilinium iodide has the layered packing. The layers, in which cations and anions alternate, are parallel to each other. In the IR spectrum of compound <b>1</b>, absorption bands at 1676 cm<sup>–1</sup>, 2949 cm<sup>–1</sup>, and 3021 cm<sup>–1</sup> correspond to C=O and C–H stretching vibrations (aliphatic and aromatic). Compound <b>1 </b>decomposes in two distinct steps. At the first step (172-200 °C), 4-acetyl-<i>N</i>,<i>N</i>,<i>N</i>-trimethylanilinium iodide decomposes with a removal of methyl iodide (i.e., inverse methylation reaction). At the second step (200-285 °C), 1-(4-(dimethylamino)phenyl)ethanon formed evaporates. Judging by the absence of the carbon residue, evaporation proceeds without decomposition.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1977 - 1984"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248267","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. E. Zazulya, P. A. Abramov, S. V. Tkachev, D. G. Sheven’, A. Yu. Komarovskikh, P. E. Plyusnin, D. B. Vasilchenko
{"title":"Structure of trans,trans-[Pt(py)2(N3)2(OH)2]·2H2O and Synthesis of Pt(IV) Prodrugs Based on It","authors":"A. E. Zazulya, P. A. Abramov, S. V. Tkachev, D. G. Sheven’, A. Yu. Komarovskikh, P. E. Plyusnin, D. B. Vasilchenko","doi":"10.1134/S0022476625090057","DOIUrl":"10.1134/S0022476625090057","url":null,"abstract":"<p>The structure of <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)<sub>2</sub>]·2H<sub>2</sub>O is studied by single crystal X-ray diffraction. The crystallographic data are: <i>a</i> = 9.8240(2) Å, <i>b</i> = 17.2178(3) Å, <i>c</i> = 9.5248(2) Å, β = 97.777(1)°, space group <i>P</i>2<sub>1</sub>/<i>c</i>, <i>Z</i> = 4, ρ<sub>cal</sub> = 2.11 g/cm<sup>3</sup>. The crystal structure of the complex consists of molecular layers perpendicular to the <i>c</i> direction. The transformation process of the dehydrate to the anhydrous complex is analyzed by thermal gravimetry. The previously published synthesis procedures of <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)(SuccH)] and <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)(Succ-NH-TEMPO)] complexes from <i>trans</i>,<i>trans</i>-[Pt(py)<sub>2</sub>(N<sub>3</sub>)<sub>2</sub>(OH)<sub>2</sub>] are modified. The optimization of synthesis conditions and the product isolation procedure increases the product yield and substantially improves the purity of the obtained compounds.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1820 - 1830"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248307","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}
P. S. Serebrennikova, A. S. Sukhikh, N. G. Naumov, S. A. Gromilov
{"title":"Tb2O3: Synthesis, Single Crystal X-Ray Diffraction Analysis, Thermal Expansion in the Range of 90-490 K","authors":"P. S. Serebrennikova, A. S. Sukhikh, N. G. Naumov, S. A. Gromilov","doi":"10.1134/S0022476625090112","DOIUrl":"10.1134/S0022476625090112","url":null,"abstract":"<p>Fine crystal samples of terbium oxide <i>C</i>-Tb<sub>2</sub>O<sub>3</sub> (space group <span>(Iabar{3})</span>, <i>Z</i> = 16) are grown from the solution-melt, which are differently colored - colorless and pale brown. No significant differences are revealed by the single crystal X-ray diffraction analysis. The unit cell parameters are refined using the external standard at <i>T</i> = 300 K with relative error Δ<i>a</i>/<i>a</i> = 2·10<sup>–5</sup>. Values <i>a</i> = 10.7302(2) Å and 10.7296(2) Å are obtained for the colorless sample and the pale brown one respectively. Dependence <i>a</i>(<i>T</i>) is studied in the range of 90-490 K for the colorless crystal. Experimental points are described by the polynomial: <i>a</i> = 10.716 + 2.7· ·10<sup>–5</sup>T + 7.2·10<sup>–8</sup>T<sup>2</sup>.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1894 - 1902"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248383","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}
V. V. Krisyuk, I. A. Baidina, I. V. Korolkov, A. E. Turgambaeva
{"title":"Structure of Heterobimetallic β-Diketonates Formed by Platinum(II) Acetylacetonate and Lead(II) Hexafluoroacetylacetonate","authors":"V. V. Krisyuk, I. A. Baidina, I. V. Korolkov, A. E. Turgambaeva","doi":"10.1134/S0022476625090161","DOIUrl":"10.1134/S0022476625090161","url":null,"abstract":"<p>New platinum(II) acetylacetonate and lead(II) hexafluoroacetylacetonate heterometallic complexes, [(Pt(acac)<sub>2</sub>)<sub>5</sub>(Pb(hfac)<sub>2</sub>)<sub>4</sub>] (<b>1</b>) and [Pt(acac)<sub>2</sub>Pb(hfac)<sub>2</sub>] (<b>2</b>), are prepared and characterized. Crystal data for <b>1</b>: <i>a</i> = 13.8795(6) Å, <i>b</i> = 15.0201(6) Å, <i>c</i> = 17.2442(7) Å, α = 105.6503(14)°, β = 110.7887(14)°, γ = 99.0552(14)°, <span>(Pbar{1})</span> space group, <i>Z</i> = 4, <i>d</i><sub>calc</sub> = 2.380 g/cm<sup>3</sup>; for <b>2</b> <i>a</i> = 16.810(6) Å, <i>b</i> = 30.960(12) Å, <i>c</i> = 18.260(7) Å, β = 105.19(2)°, <i>C</i>2/<i>c</i> space group, <i>Z</i> = 16, <i>d</i><sub>calc</sub> = 2.204 g/cm<sup>3</sup>. The main structural motifs of these compounds are same-type 1D coordination polymers stabilized by Pt⋯Pt and Pb–O contacts.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1942 - 1950"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248270","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":"Structure of a New Phase of a Volatile Platinum(II) Complex with 1,1,1-Trifluoro-4-Iminopentan-2-One","authors":"I. A. Baidina, N. V. Pervukhina, S. A. Gromilov","doi":"10.1134/S0022476625090021","DOIUrl":"10.1134/S0022476625090021","url":null,"abstract":"<p>The structure of a new phase of a volatile Pt(ktf)<sub>2</sub> complex, where ktf = CF<sub>3</sub>–C(O)–CH–C(NH)–CH<sub>3</sub>, is determined by single crystal X-ray diffraction. The crystallographic data for C<sub>10</sub>H<sub>10</sub>F<sub>6</sub>N<sub>2</sub>O<sub>2</sub>Pt are as follows: <i>a</i> = 12.1716(7) Å,<i> b</i> = 8.5581(7) Å,<i> c</i> = 19.9966(15) Å, β = 96.840(3)°, space group <i>P</i>2<sub>1</sub>/<i>c</i>, <i>Z</i> = 6,<i> R</i> = 0.046. The compound is a 2:1 mixture of <i>cis</i>- and <i>trans</i>-isomers. The square environment of the platinum atom consists of oxygen and nitrogen atoms of two bidentately bonded ketoiminate ligands, resulting in the PtO<sub>2</sub>N<sub>2</sub> coordination core. The difference in Pt–O (2.005 Å) and Pt–N (1.990 Å) bond lengths is 0.015 Å in the <i>trans</i>-isomer; the O–Pt–N chelate angle is 93.6°. In the <i>cis</i>-isomer, the average Pt–O and Pt–N bond lengths are 2.002 Å and 1.967 Å respectively; the chelate angle is 94.8°. The molecules are packed into infinite stacks with Pt⋯Pt distances of 4.096 Å and 4.159 Å.</p>","PeriodicalId":668,"journal":{"name":"Journal of Structural Chemistry","volume":"66 9","pages":"1786 - 1796"},"PeriodicalIF":1.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145248271","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}