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Structural Features of Tetra(p-tolyl)antimony p-Tol4SbX (X = Br, OC(O)Ph ∙ PhH, OSO2C6H2Me3-2,4,6) Derivatives 四(对甲苯)锑 p-Tol4SbX (X = Br, OC(O)Ph ∙ PhH, OSO2C6H2Me3-2,4,6) 的结构特征衍生物
Pub Date : 2024-03-20 DOI: 10.1134/s2634827624600026
V. V. Sharutin

Abstract

The structure of the tetra(p-tolyl)antimony compounds p-Tol4SbX (X = Br (1), OC(O)Ph ∙ PhH (2), OSO2C6Me3-2,4,6 (3)) is determined by X-ray diffraction analysis (XRD). According to the XRD data, the antimony atoms in complexes 13 exhibit a distorted trigonal bipyramidal coordination with three aryl ligands in the equatorial plane, and the axial angles CSbX are 174.75(8)°, 175.13(9)°, and 174.51(6)°, respectively.

The XRD data for compound 1 are as follows: C28H28BrSb, M = 566.16; monoclinic system, sp. gr. P21/n; cell parameters: a = 9.868(6) Å, b = 23.312(11) Å, c = 12.106(6) Å; β = 113.15(2)°, V = 2561(2) Å3, Z = 4; ρ(calc.) = 1.469 g/cm3; μ = 2.649 mm–1; F(000) = 1128.0; 2θ data acquisition region: 6.4°–56.76°; –13 ≤ h ≤ 13, –31 ≤ k ≤ 31, –16 ≤ l ≤ 16; total reflections 42 998; independent reflections 6359 (Rint = 0.0346); GOOF = 1.080; R factor 0.0325. For compound 2: C41H39O2Sb, M = 685.47; monoclinic system, sp. gr. С2/с; cell parameters: a = 28.186(13) Å, b = 15.116(6) Å, c = 17.629(8) Å; β = 91.73(2)°, V = 7507(6) Å3, Z = 8; ρ(calc.) = 1.213 g/cm3; μ = 0.765 mm–1; F(000) = 2816,0; 2θ data acquisition region: 6.572°–56.996°; –37 ≤ h ≤ 37, –20 ≤ k ≤ 20, –23 ≤ l ≤ 23; total reflections 116 806; independent reflections 9489 (Rint = 0.0492); GOOF = 1.102; R factor 0.0363. For compound 3: C37H39O3SSb, M = 685.49; monoclinic system, sp. gr. P21/n; cell parametrs: a = 12.172(4) Å, b = 18.802(5) Å, c = 15.433(6) Å; β = 108.744(12)°, V = 3345(2) Å3, Z = 4; ρ(calc.) = 1.361 g/cm3; μ = 0.921 mm–1; F(000) = 1408.0; 2θ data acquisition region: 5.96°–63.02°; –16 ≤ h ≤ 17, –27 ≤ k ≤ 27, ‒22 ≤ l ≤ 21; total reflections 138 835; independent reflections 11 081 (Rint = 0.0373); GOOF = 1.045; R factor 0.0304. Complete tables of atomic coordinates, bond lengths, and bond angles for compounds 13 have been deposited to the Cambridge Structural Database (CSD) with the following deposition numbers: 2182608, 2149953, and 2171918. For access to the data, please contact deposit@ccdc.cam.ac.uk or visit http://www.ccdc.cam.ac.uk.

摘要 通过 X 射线衍射分析(XRD)确定了四(对甲苯基)锑化合物 p-Tol4SbX(X = Br (1),OC(O)Ph ∙ PhH (2),OSO2C6Me3-2,4,6 (3))的结构。根据 XRD 数据,配合物 1-3 中的锑原子与三个芳基配体在赤道面上呈现出畸变的三叉双锥配位,轴角 CSbX 分别为 174.75(8)°、175.13(9)° 和 174.51(6)°:化合物 1 的 XRD 数据如下:C28H28BrSb,M = 566.16;单斜体系,sp.gr. P21/n;晶胞参数:a = 9.868(6) Å,b = 23.312(11) Å,c = 12.106(6) Å;β = 113.15(2)° ,V = 2561(2) Å3 ,Z = 4 ;ρ(calc. ) = 1.469 g/cm3 ;μ = 2.649 mm-1 ;F(000) = 1128.0;2θ 数据采集区域:6.4°-56.76°;-13 ≤ h ≤ 13,-31 ≤ k ≤ 31,-16 ≤ l ≤ 16;总反射 42 998;独立反射 6359(Rint = 0.0346);GOOF = 1.080;R 因子 0.0325。化合物 2:C41H39O2Sb,M = 685.47;单斜体系,sp.С2/с; 晶胞参数:a = 28.186(13) Å, b = 15.116(6) Å, c = 17.629(8) Å; β = 91.73(2)°, V = 7507(6) Å3, Z = 8; ρ(calc.) = 1.213 g/cm3; μ = 0.765 mm-1; F(000) = 2816,0; 2θ 数据采集区域:6.572°-56.996°; -37 ≤ h ≤ 37, -20 ≤ k ≤ 20, -23 ≤ l ≤ 23; 总反射 116 806; 独立反射 9489 (Rint = 0.0492); GOOF = 1.102; R 因子 0.0363。化合物 3:C37H39O3SSb,M = 685.49;单斜体系,sp. gr. P21/n;晶胞参数:a = 12.172(4)埃,b = 18.802(5)埃,c = 15.433(6) Å; β = 108.744(12)°, V = 3345(2) Å3, Z = 4; ρ(calc.) = 1.361 g/cm3; μ = 0.921 mm-1; F(000) = 1408.0; 2θ 数据采集区域:5.96°-63.02°;-16 ≤ h ≤ 17,-27 ≤ k ≤ 27,-22 ≤ l ≤ 21;总反射 138 835;独立反射 11 081(Rint = 0.0373);GOOF = 1.045;R 因子 0.0304。化合物 1-3 的原子坐标、键长和键角的完整表格已存入剑桥结构数据库 (CSD),存入编号如下:2182608、2149953 和 2171918。如需访问这些数据,请联系 deposit@ccdc.cam.ac.uk 或访问 http://www.ccdc.cam.ac.uk。
{"title":"Structural Features of Tetra(p-tolyl)antimony p-Tol4SbX (X = Br, OC(O)Ph ∙ PhH, OSO2C6H2Me3-2,4,6) Derivatives","authors":"V. V. Sharutin","doi":"10.1134/s2634827624600026","DOIUrl":"https://doi.org/10.1134/s2634827624600026","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>The structure of the tetra(<i>p</i>-tolyl)antimony compounds <i>p</i>-Tol<sub>4</sub>SbX (X = Br (<b>1</b>), OC(O)Ph ∙ PhH (<b>2</b>), OSO<sub>2</sub>C<sub>6</sub>Me<sub>3</sub>-2,4,6 (<b>3</b>)) is determined by X-ray diffraction analysis (XRD). According to the XRD data, the antimony atoms in complexes <b>1</b>–<b>3</b> exhibit a distorted trigonal bipyramidal coordination with three aryl ligands in the equatorial plane, and the axial angles CSbX are 174.75(8)°, 175.13(9)°, and 174.51(6)°, respectively.</p><p>The XRD data for compound <b>1</b> are as follows: C<sub>28</sub>H<sub>28</sub>BrSb, <i>M</i> = 566.16; monoclinic system, sp. gr. <i>P</i>2<sub>1</sub>/<i>n</i>; cell parameters: <i>a</i> = 9.868(6) Å, <i>b</i> = 23.312(11) Å, <i>c =</i> 12.106(6) Å; β = 113.15(2)°, <i>V</i> = 2561(2) Å<sup>3</sup>, <i>Z</i> = 4; ρ(calc.) = 1.469 g/cm<sup>3</sup>; μ = 2.649 mm<sup>–1</sup>; <i>F</i>(000) = 1128.0; 2θ data acquisition region: 6.4°–56.76°; –13 ≤ <i>h</i> ≤ 13, –31 ≤ <i>k</i> ≤ 31, –16 ≤ <i>l</i> ≤ 16; total reflections 42 998; independent reflections 6359 (<i>R</i><sub>int</sub> = 0.0346); GOOF = 1.080; <i>R</i> factor 0.0325. For compound <b>2</b>: C<sub>41</sub>H<sub>39</sub>O<sub>2</sub>Sb, <i>M</i> = 685.47; monoclinic system, sp. gr. <i>С</i>2/<i>с</i>; cell parameters: <i>a</i> = 28.186(13) Å, <i>b</i> = 15.116(6) Å, <i>c =</i> 17.629(8) Å; β = 91.73(2)°, <i>V</i> = 7507(6) Å<sup>3</sup>, <i>Z</i> = 8; ρ(calc.) = 1.213 g/cm<sup>3</sup>; μ = 0.765 mm<sup>–1</sup>; <i>F</i>(000) = 2816,0; 2θ data acquisition region: 6.572°–56.996°; –37 ≤ <i>h</i> ≤ 37, –20 ≤ <i>k</i> ≤ 20, –23 ≤ <i>l</i> ≤ 23; total reflections 116 806; independent reflections 9489 (<i>R</i><sub>int</sub> = 0.0492); GOOF = 1.102; <i>R</i> factor 0.0363. For compound <b>3</b>: C<sub>37</sub>H<sub>39</sub>O<sub>3</sub>SSb, <i>M</i> = 685.49; monoclinic system, sp. gr. <i>P</i>2<sub>1</sub>/<i>n</i>; cell parametrs: <i>a</i> = 12.172(4) Å, <i>b</i> = 18.802(5) Å, <i>c =</i> 15.433(6) Å; β = 108.744(12)°, <i>V</i> = 3345(2) Å<sup>3</sup>, <i>Z</i> = 4; ρ(calc.) = 1.361 g/cm<sup>3</sup>; μ = 0.921 mm<sup>–1</sup>; <i>F</i>(000) = 1408.0; 2θ data acquisition region: 5.96°–63.02°; –16 ≤ <i>h</i> ≤ 17, –27 ≤ <i>k</i> ≤ 27, ‒22 ≤ <i>l</i> ≤ 21; total reflections 138 835; independent reflections 11 081 (<i>R</i><sub>int</sub> = 0.0373); GOOF = 1.045; <i>R</i> factor 0.0304. Complete tables of atomic coordinates, bond lengths, and bond angles for compounds <b>1</b>–<b>3</b> have been deposited to the Cambridge Structural Database (CSD) with the following deposition numbers: 2182608, 2149953, and 2171918. For access to the data, please contact deposit@ccdc.cam.ac.uk or visit http://www.ccdc.cam.ac.uk.</p>","PeriodicalId":21086,"journal":{"name":"Reviews and Advances in Chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140167515","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}
引用次数: 0
Synthesis Methods, Structure, and Applications of Metal Dicyanoaurate, Tetracyanoaurate, and Dihalodicyanoaurate Complexes 二氰基金酸酯、四氰基金酸酯和二卤代二氰基金酸酯金属配合物的合成方法、结构和应用
Pub Date : 2024-03-20 DOI: 10.1134/s2634827624600051
D. P. Shevchenko

Abstract

Cyanoaurate complexes represent a broad class of compounds with diverse structures. In particular, coordination polymers based on these complexes have numerous potential practical applications, including in microelectronics, nanotechnology, materials science, and medicine. In the development of new functional materials, significant attention is given to the possibility of molecules and other structural units participating in noncovalent interactions, which play a crucial role in determining the physicochemical properties and biological activity of these materials. Thus, the presence of aurophilic contacts or halogen–halogen interactions in cyanoaurate complexes only intensifies researchers’ interest in this class of compounds. At present, study of the chemistry of gold cyanides continues to develop rapidly, making the synthesis and exploration of new cyanoaurate compounds, as well as the systematization of the knowledge gained, relevant tasks. This review, encompassing a description of contemporary achievements in the methods of synthesis, investigation of structural features, and potential practical applications of metal dicyanoaurates, tetracyanoaurates, and dihalodicyanoaurates of both molecular and ionic types, is based on an analysis of publications, with the majority of sources published before 2022. Some more recent studies are also included in the review. The information presented in this article is fundamentally important and undoubtedly valuable for specialists in the field of inorganic and organometallic chemistry of gold.

摘要 金牛酸盐配合物是一类结构多样的化合物。特别是基于这些配合物的配位聚合物具有许多潜在的实际应用,包括微电子学、纳米技术、材料科学和医学。在开发新功能材料的过程中,分子和其他结构单元参与非共价相互作用的可能性受到了极大关注,这种相互作用在决定这些材料的理化性质和生物活性方面起着至关重要的作用。因此,氰基金酸酯复合物中存在亲欧接触或卤素-卤素相互作用,只会增强研究人员对这一类化合物的兴趣。目前,对氰化金化学的研究仍在迅速发展,因此合成和探索新的氰基金酸酯化合物以及将所获得的知识系统化是一项重要任务。本综述基于对出版物的分析,其中大部分资料发表于 2022 年之前,介绍了当代在分子和离子型金属二氰基金酸盐、四氰基金酸盐和二卤代二氰基金酸盐的合成方法、结构特征研究和潜在实际应用方面取得的成就。一些较新的研究也包含在综述中。本文所提供的信息对于金的无机化学和有机金属化学领域的专家来说,无疑是非常重要和有价值的。
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引用次数: 0
Synthesis of 2-Phenyl-1,3-Oxazoles, 2-Imidazolinones, and 2-Imidazolinthiones Containing a Diterpene Fragment 含二萜片段的 2-苯基-1,3-恶唑、2-咪唑啉酮和 2-咪唑啉酮的合成
Pub Date : 2024-03-20 DOI: 10.1134/s2634827624600014
R. M. Sultanova, G. Z. Kuleshina, N. S. Khusnutdinova

Abstract

The report describes the synthesis of a series of new imidazolinones-2, imidazole-2-thiones, and 1,3-oxazoles based on the interaction of 1-bromo ketones containing a diterpene fragment with urea and thiourea. It is shown that the direction of the reaction and the yields of the products depend on the nature of the initial substrates and the conditions of the reaction. For instance, boiling bromides with ureas or thiourea in ethyl alcohol in the presence of sodium carbonate leads to nucleophilic substitution, forming diterpene-substituted ureas. Performing the same reaction in ethylene glycol at a temperature of 200–250°C in the presence of potassium hydroxide results in the formation of imidazolin-2-ones or -thiones containing the diterpene fragment at the 4-position with high yields.

摘要 本报告介绍了基于含有二萜片段的 1-溴酮与脲和硫脲的相互作用,合成一系列新的咪唑啉酮-2、咪唑-2-硫酮和 1,3-恶唑。研究表明,反应的方向和产物的产量取决于初始底物的性质和反应条件。例如,在碳酸钠存在下,将溴化物与脲或硫脲在乙醇中煮沸,会发生亲核取代反应,生成二萜取代的脲。在有氢氧化钾存在的情况下,在 200-250°C 的乙二醇温度下进行相同的反应,会以高产率生成在 4 位含有二萜片段的咪唑啉-2-酮或-硫酮。
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引用次数: 0
Spectrophotometric Investigation of the Reaction of Cu(II) Ions with N-Benzoyl-N'-(phenylsulphonyl)hydrazine in Ammonia Media 氨介质中 Cu(II)离子与 N-苯甲酰基-N'-(苯基磺酰基)肼反应的分光光度法研究
Pub Date : 2024-02-28 DOI: 10.1134/s2634827623600160
Yu. B. Elchishcheva, A. S. Sorokina, P. T. Pavlov

Abstract

We investigated the complexation reaction of N-benzoyl-N'-(phenylsulfonyl)hydrazine with Cu(II) ions in an ammonia medium. The absorption spectra of the reagent and its complex compound with Cu(II) ions were recorded and analyzed. Optimal conditions for complex formation were determined, including the pH range for complexation, the optimal time for color development, and the amount of photometric reagent. Under optimal conditions, a calibration curve for the complexation of BFSH with Cu(II) ions was plotted. The Beer–Lambert–Bouguer law is valid in the range from 0.5 to 1.75 mg of Cu(II) in 25 mL of the solution. The true (19 389 cm2/mol) and apparent (4708 cm2/mol) molar absorption coefficients were calculated. Using the methods of saturation, equilibrium shift, curve intersection, isomolar series, and conductometric titration, the molar ratios in the solution of the complex compound were determined as [Cu(II)] : [BFSH] = 1 : 1 and 1 : 2. The conditional stability constant of the complex, calculated using the Babko method, is 2.45 × 1013. The convergence and accuracy of the spectrophotometric method were determined statistically.

摘要 我们研究了 N-苯甲酰基-N'-(苯磺酰基)肼与 Cu(II)离子在氨介质中的络合反应。记录并分析了试剂及其与 Cu(II) 离子的络合物的吸收光谱。确定了络合物形成的最佳条件,包括络合的 pH 值范围、显色的最佳时间以及光度测定试剂的用量。在最佳条件下,绘制出了 BFSH 与 Cu(II) 离子络合的校准曲线。比尔-朗伯-布格尔定律在 25 毫升溶液中含 0.5 至 1.75 毫克 Cu(II)的范围内有效。计算了真实摩尔吸收系数(19 389 cm2/mol)和表观摩尔吸收系数(4708 cm2/mol)。利用饱和、平衡移动、曲线相交、等摩尔数列和电导滴定等方法,确定了复合物溶液中的摩尔比为 [Cu(II)] : [BFSH] = 1 : 1 和 1 : 2。用巴布科方法计算出的该复合物的条件稳定常数为 2.45 × 1013。分光光度法的收敛性和准确性是通过统计学方法确定的。
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引用次数: 0
Prospective Components of Rocket Propellant. I. Oxidizers 火箭推进剂的预期成分。I. 氧化剂
Pub Date : 2024-02-28 DOI: 10.1134/s2634827623600147
A. L. Vereshchagin

Abstract

The review focuses on the latest advancements in chlorine-free oxidizers for solid rocket propellants as of January 1, 2023. The properties and applications of phase-stabilized ammonium nitrate, ammonium dinitramide, and compounds with trinitromethyl and trinitroethyl groups as high-density explosive materials, plasticizers, and components of solid rocket propellants are discussed. Formulations of rocket propellants containing these components, along with their physicomechanical properties, ballistic characteristics, and chemical stability indicators, are presented.

摘要 本综述重点介绍截至 2023 年 1 月 1 日用于固体火箭推进剂的无氯氧化剂的最新进展。文章讨论了相稳定硝酸铵、二硝化铵以及含有三硝基甲基和三硝基乙基的化合物作为高密度爆炸材料、增塑剂和固体火箭推进剂成分的特性和应用。介绍了含有这些成分的火箭推进剂的配方及其物理机械性能、弹道特性和化学稳定性指标。
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引用次数: 0
Physical and Chemical Properties of Oxalic Acid N'-Tosylhydrazide Ethyl Ether 草酸 N'-对甲苯磺酸肼乙醚的物理和化学特性
Pub Date : 2024-02-28 DOI: 10.1134/s2634827623600159
Yu. B. Elchishcheva, O. A. Posokhina, P. T. Pavlov

Abstract

We present the results of the investigation of the physicochemical properties of oxalic acid N'-tosylhydrazide ethyl ester (THE). The solubility of the reagent was examined in ethanol, 0.1 mol/L KOH solution, toluene, chloroform, hexane, and water using spectrophotometry, refractometry, and gravimetry. The results suggest that THE can be useful in flotation and extraction processes. Acid–base equilibria in the reagent solutions were studied by spectrophotometric methods. The obtained dissociation constants (pKa1 = 7.56 ± 0.14; pKa2 = 13.48 ± 0.22) confirm that THE is a weak dibasic acid. The hydrolytic stability of the reagent was investigated spectrophotometrically. The research findings indicate that THE solutions are sufficiently stable over time in alkaline media, with a hydrolysis rate of 4.77% over 2 h. The surface activity of the reagent was determined by the stalagmometric method, revealing that THE is a surfactant.

摘要 我们展示了草酸 N'-tosylhydrazide 乙酯(THE)的理化性质研究结果。采用分光光度法、折光法和重量法检测了该试剂在乙醇、0.1 mol/L KOH 溶液、甲苯、氯仿、正己烷和水中的溶解度。结果表明,THE 可用于浮选和萃取过程。通过分光光度法研究了试剂溶液中的酸碱平衡。得到的解离常数(pKa1 = 7.56 ± 0.14;pKa2 = 13.48 ± 0.22)证实 THE 是一种弱二元酸。分光光度法研究了该试剂的水解稳定性。研究结果表明,THE 溶液在碱性介质中具有足够的稳定性,2 小时内的水解率为 4.77%。
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引用次数: 0
Review of Recent Advances in the Use of Drug Delivery Systems in Ophthalmology 眼科用给药系统的最新进展回顾
Pub Date : 2024-02-28 DOI: 10.1134/s2634827623600081
Dmitriy Berillo, Baurzhan Kadyrgaliev

Abstract

Eye drops represent the traditional form of medication delivery for the eyes, constituting approximately 90% of the presently available ophthalmic formulations. While they are generally well-received by patients, a significant challenge associated with eye drops is the rapid loss of medication before it reaches the cornea. The creation of new systems and means of drug delivery is important for solving the main problems of medicine – improving the therapeutic efficiency, tolerability, and safety of medical therapy. In the treatment of numerous of eye diseases, the main problem is creating a constant and sufficient concentration of drugs in the lesion due to the peculiarities of the anatomical and physiological structure of the eyeball. New approaches to non-invasive drug delivery are being developed, such as eye implants, contact lenses, as well as drug delivery systems based on nanoparticles, micelles, dendrimers, microneedles and liposomes. In situ gelation systems are also the subject of study and promising developments. Combining drugs within conventional delivery systems has the potential to pave the way for enhanced outcomes and improved therapeutic responses, particularly for systems that have previously shown limited effectiveness. This review discusses current understanding and recent discoveries attributed the utilisation of drug delivery systems in ophthalmology, including the characteristics, advantages, and disadvantages of each class of delivery system.

摘要 眼药水是传统的眼部给药方式,约占目前眼科制剂的 90%。虽然滴眼液普遍受到患者的欢迎,但滴眼液面临的一个重大挑战是药物在到达角膜之前会迅速流失。创造新的给药系统和方法对于解决医学的主要问题--提高治疗效率、耐受性和安全性--非常重要。由于眼球解剖和生理结构的特殊性,在治疗许多眼科疾病时,主要问题是在病变部位形成恒定和足够的药物浓度。目前正在开发的非侵入性给药新方法包括眼部植入物、隐形眼镜以及基于纳米颗粒、胶束、树枝状聚合物、微针和脂质体的给药系统。原位凝胶系统也是研究的主题,发展前景广阔。在传统给药系统中结合使用药物有可能为提高疗效和改善治疗反应铺平道路,特别是对于以前显示出有限有效性的系统。本综述讨论了目前对眼科用给药系统的理解和最新发现,包括各类给药系统的特点、优点和缺点。
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引用次数: 0
Quinoline-Containing π-Conjugated Systems: Synthesis, Research, and Application of Quinophthalone Dyes 含喹啉的π-共轭体系:喹酞酮染料的合成、研究和应用
Pub Date : 2024-02-28 DOI: 10.1134/s2634827623600196
E. V. Shklyaeva, A. V. Ozhgikhina, G. G. Abashev

Abstract

Here we present the literary review concerning methods of synthesis and application fields of substituted quinophthalones, an interesting class of heterocyclic compounds containing fragments of substituted/unsubstituted quinolines and phthalic anhydride in their structure. Such compounds have an extended π-conjugated system and are, therefore, most often used as dyes.

摘要 我们在此介绍有关取代喹酞酮的合成方法和应用领域的文献综述。取代喹酞酮是一类有趣的杂环化合物,其结构中含有取代/未取代喹啉和邻苯二甲酸酐的片段。这类化合物具有扩展的 π 共轭体系,因此最常用作染料。
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引用次数: 0
Reactions of Pentaphenyl- and Penta(para-tolyl)antimony with Ferrocenedicarboxylic Acid 五苯基和五(对位甲苯基)锑与二茂铁二羧酸的反应
Pub Date : 2024-02-28 DOI: 10.1134/s2634827623600184
V. V. Sharutin

Abstract

Interaction of pentafluorophenyl- and penta(para-tolyl)antimony with ferrocenedicarboxylic acid (molar ratios 1 : 1 and 2 : 1) in toluene (20°C, 24 h) results in the substitution of hydrogen in one or two carboxylate groups, leading to the formation of ferrocenecarboxylates of tetraaryl antimony HOOCС5H4FeС5H4C(O)OSbPh4 (1), HOOCС5H4FeС5H4C(O)OSbTol4 (2), Ph4SbC(O)OС5H4FeС5H4C(O)OSbPh4 (3) and p-Tol4SbC(O)OС5H4FeС5H4C(O)OSbTol4 (4) with yields up to 83%. Compounds 14 were identified by elemental analysis, IR spectroscopy, and X-ray diffraction analysis for 4. The XRD analysis of complex 4 was conducted on an a D8 Quest Bruker automatic four-circle diffractometer (Мо Kα radiation, λ = 0,71073 Å, graphite monochromator) at 293 K. Crystallographic characteristics of 4: monoclinic syngony, space group P21/c, a = 17.227(17) Å, b = 11.064(9) Å, c = 30.59(3) Å, β = 100.00(4)°, V = 5742(9) Å3, Z = 4, ρcalc = 1.440 g/cm3, 2θ 6.02°−49.08°, 124 343 total reflections, 9436 independent reflections, number of refined parameters 684, Rint = 0.1051, GOOF 1.094, R1 = 0.0536, wR2 = 0.1309, residual electron density (max/min) 0.88/–1.21 e/Å3. According to XRD analysis, the coordination of antimony atoms in crystal 4 is distorted octahedral due to the bidentate chelating nature of the carboxylate ligand. Diagonal angles in the two octahedra are 146.4(2)°, 154.0(3)°, 171.0(2)° and 147.4(2)°, 154.8(2)°, 166.9(2)°. The Sb−О distances are 2.296(5), 2.502(5) Å and 2.289(5), 2.453(5) Å, while the Sb−С bonds differ significantly, 2.146(7)−2.166(7) and 2.123(6)−2.165(7) Å. The structural organization of the crystal is mainly governed by С−Н···π interactions.

摘要五氟苯锑和五对甲苯锑与二茂铁羧酸(摩尔比为 1 : 1 和 2 :在甲苯中(20°C,24 小时),一个或两个羧酸基团中的氢被取代,形成四芳基锑的二茂铁羧酸盐 HOOCС5H4FeС5H4C(O)OSbPh4(1)、HOOCС5H4FeС5H4C(O)OSbTol4 (2)、Ph4SbC(O)OС5H4FeС5H4C(O)OSbPh4 (3) 和 p-Tol4SbC(O)OС5H4FeС5H4C(O)OSbTol4 (4),收率高达 83%。化合物 1-4 通过元素分析、红外光谱和 4 的 X 射线衍射分析进行了鉴定。复合物 4 的 X 射线衍射分析是在一台 D8 Quest Bruker 自动四圆衍射仪(Мо Kα 辐射,λ = 0,71073 Å,石墨单色器)上进行的,温度为 293 K。4 的晶体学特征:单斜共晶,空间群 P21/c,a = 17.227(17) Å,b = 11.064(9) Å,c = 30.59(3) Å, β = 100.00(4)°, V = 5742(9) Å3, Z = 4, ρcalc = 1.440 g/cm3, 2θ 6.02°-49.08°, 124 343 个总反射,9436 个独立反射,精炼参数数 684, Rint = 0.1051,GOOF 1.094,R1 = 0.0536,wR2 = 0.1309,残余电子密度(最大/最小)0.88/-1.21 e/Å3。根据 XRD 分析,由于羧酸配体的双齿螯合性质,晶体 4 中锑原子的配位为畸变八面体。两个八面体的对角分别为 146.4(2)°、154.0(3)°、171.0(2)° 和 147.4(2)°、154.8(2)°、166.9(2)°。晶体的结构组织主要受 С-Н---π 相互作用的支配。
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引用次数: 0
Photoinduced Increase in the Conjugation Length of Polymer Chains in Blue-Phase Polydiacetylene Films based on Diacetylene Alcohol Derivatives 光诱导增加基于二乙炔醇衍生物的蓝相聚二乙炔薄膜中聚合物链的共轭长度
Pub Date : 2024-02-28 DOI: 10.1134/s263482762360010x
A. S. Alekseev, A. B. Ivanov, V. V. Klechkovskaya, M. S. Lukasov, R. M. Sarimov, T. O. Teplyakova

Abstract

Photoinduced polymerization of Langmuir–Schaefer monolayers of four unsymmetrical hydroxyalkadiynyl N-arylcarbamate derivatives, prepared on the basis of diynes solutions with an extremely low concentration, was studied under prolonged UV irradiation. The kinetics of these diacetylene (DA) molecules films transition to the blue phase of polydiacetylenes (PDA) films, which is not characteristic of any other DA alcohol derivatives, has been studied by light absorption spectroscopy and scanning electron microscopy. The structure homogeneity of DA and PDA films was demonstrated. A continuous shift of the optical absorption band of each PDA film to the long-wavelength region of the spectrum during 60 min of UV light irradiation was found. That indicated an increase of the chains conjugation length in blue-phase PDA samples.

摘要 在长时间紫外线照射下,研究了以浓度极低的二炔溶液为基础制备的四种不对称羟基烷二炔 N-芳基氨基甲酸酯衍生物的朗缪尔-谢弗单层的光诱导聚合。通过光吸收光谱学和扫描电子显微镜研究了这些二乙炔(DA)分子薄膜过渡到聚二乙烯(PDA)薄膜蓝相的动力学,这是其他任何二乙炔醇衍生物所不具备的。结果表明,DA 和 PDA 薄膜的结构是均匀的。在紫外光照射 60 分钟期间,发现每种 PDA 薄膜的光吸收带持续向光谱的长波长区移动。这表明蓝相 PDA 样品的链共轭长度增加了。
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引用次数: 0
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Reviews and Advances in Chemistry
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