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Zn(II) complex with pyridine based 1,3-selenazolyl-hydrazone: Synthesis, structural characterization and DFT study 吡啶基1,3-硒化偶氮腙配合物Zn(II)的合成、结构表征及DFT研究
4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230831079a
Jovana Araskov, Predrag Ristic, Aleksandar Visnjevac, Andrej Milivojac, Dragana Mitic, Nenad Filipovic, Tamara Todorovic
An octahedral complex of Zn(II) with a ligand from a class of pyridine-based 1,3-selenazolyl-hydrazones was synthesized and characterized by IR and NMR spectroscopy and single crystal X-ray diffraction analysis. The purity of the complex was confirmed by elemental analysis. Two ligands are coordinated in the neutral NNN-tridentate form forming a complex cation, while the positive charge is neutralized by [ZnCl4]2-. Complex crystallizes in monoclinic C2/c space group with the Zn atoms situated in a special position. The packing features of the novel complex were analyzed using Hirshfeld surfaces, construction of 2D pseudosymmetric plot and DFT quantum mechanical calculations and compared with the previously published sulfur-based isostere. The key difference in the structures, imposed by replacement of sulfur with selenium, were identified.
合成了锌(II)与一类吡啶类1,3-硒化偶氮腙配体的八面体配合物,并用红外、核磁共振和单晶x射线衍射对其进行了表征。通过元素分析证实了该配合物的纯度。两个配体以中性的nnn -三齿状配位形成络合阳离子,而正电荷被[ZnCl4]2-中和。配合物在单斜C2/c空间群中结晶,锌原子位于特殊位置。利用Hirshfeld曲面、二维伪对称图的构造和DFT量子力学计算分析了新型配合物的填充特征,并与先前发表的硫基等分体进行了比较。在结构上的关键区别是由硒取代硫造成的。
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引用次数: 0
Synthesis and structural analysis of tetranuclear Zn(II) complex with 2,3-dihydroxybenzaldehyde-aminoguanidine 2,3-二羟基苯甲醛-氨基胍四核配合物Zn(II)的合成及结构分析
4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230808067k
Marijana Kostic, Marko Rodic, Ljiljana Vojinovic-Jesic, Mirjana Radanovic
Here we report a new Schiff base of aminoguanidine and 2,3- dihydroxybenzaldehyde (H2L) and its physicochemical characterization, along with an investigation into its coordination affinities towards zinc. By reacting zinc acetate with the chloride salt of the ligand in the MeCN-H2O solution, yellow single-crystals of tetranuclear, centrosymmetric complex, with the formula [Zn2(?-L)(?-OAc)2]2?2MeCN, were obtained. The complex was characterized by IR spectroscopy, conductometry, elemental analysis, and single-crystal X-ray diffraction analysis. Notably, both nitrogen atoms of the aminoguanidine residue coordinate to the same zinc atom, while both deprotonated phenyl oxygen atoms achieve bridging coordination. Furthermore, two acetate anions bridge adjacent zinc atoms in addition to the Schiff base anion. Meaningful insights into the hierarchy and significance of intermolecular interactions within the crystal structure were gained by estimating the energies using the CrystalExplorer model. The calculations revealed that the crystal structure can be classified as a layer type, with notably stronger interactions occurring along the [0 0 1] and [0 1 1] directions.
本文报道了一种新的氨基胍和2,3-二羟基苯甲醛(H2L)希夫碱及其理化性质,并对其与锌的配位亲和力进行了研究。在men - h2o溶液中,醋酸锌与配体的氯盐反应,得到四核中心对称络合物的黄色单晶,式为[Zn2(?-L)(?-OAc)2]2?得到2MeCN。通过红外光谱、电导、元素分析和单晶x射线衍射分析对配合物进行了表征。值得注意的是,氨基胍残基的两个氮原子都配位到同一个锌原子上,而两个去质子化的苯基氧原子都实现了桥接配位。此外,除了席夫碱阴离子外,还有两个醋酸阴离子桥接相邻的锌原子。通过使用CrystalExplorer模型估计能量,获得了对晶体结构中分子间相互作用的层次和意义的有意义的见解。计算表明,晶体结构可归类为层型,沿[0 0 1]和[0 11 1]方向发生明显更强的相互作用。
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引用次数: 0
Structure and DNA/BSA binding study of zinc(II) complex with 4-ethynyl-2,2’-bipyridine 4-乙基-2,2′-联吡啶配合物锌(II)的结构及DNA/BSA结合研究
4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230605066a
Tina Andrejevic, Darko Asanin, Aurélien Crochet, Nevena Stevanovic, Ivana Vucenovic, Fabio Zobi, Milos Djuran, Biljana Glisic
In the present study, a zinc(II) complex with 4-ethynyl-2,2?-bipyridine (ebpy), [Zn(ebpy)Cl2], was synthesized and characterized by spectroscopic (1H NMR, IR and UV-Vis) methods and molar conductivity measurement. The crystal structure of the [Zn(ebpy)Cl2] complex was determined by single-crystal X-ray diffraction analysis, confirming the bidentate coordination of the ebpy ligand through its two nitrogen atoms, while the remaining two coordination sites are occupied by two chloride ions. With the aim to investigate the reactivity of the synthesized zinc(II) complex toward biologically important molecules, its binding affinity to calf thymus DNA (ct-DNA) and bovine serum albumin (BSA) was studied by fluorescence emission spectroscopy. From the obtained results, it can be concluded that [Zn(ebpy)Cl2] complex binds to BSA reversibly, while the combination of ethidium bromide (EthBr) and Hoechst 33258 (2?-(4-hydroxyphenyl)-5-[5-(4-methylpiperazine- 1-yl)benzimidazo-2-yl]-benzimidazole) competitive binding study suggests that this complex interacts with ct-DNA through the minor groove binding, which is in agreement with molecular docking study.
在本研究中,锌(II)配合物与4-乙基-2,2?合成了-联吡啶(ebpy), [Zn(ebpy)Cl2],并采用波谱(1H NMR, IR和UV-Vis)方法和摩尔电导率测量对其进行了表征。通过单晶x射线衍射分析确定了[Zn(ebpy)Cl2]配合物的晶体结构,证实了ebpy配体通过其两个氮原子进行双齿配位,而其余两个配位被两个氯离子占据。为了研究合成的锌(II)配合物对重要生物分子的反应性,利用荧光发射光谱研究了其与小牛胸腺DNA (ct-DNA)和牛血清白蛋白(BSA)的结合亲和力。从得到的结果可以得出,[Zn(ebpy)Cl2]配合物与BSA的结合是可逆的,而溴化乙啶(EthBr)与Hoechst 33258(2?-(4-羟基苯基)-5-[5-(4-甲基哌嗪- 1-基)苯并咪唑-2-基]苯并咪唑)的竞争结合研究表明,该配合物与ct-DNA的相互作用是通过轻微的凹槽结合,这与分子对接研究一致。
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引用次数: 0
Spectroscopic and structural characterization of hexaamminecobalt(III) dibromide permanganate 二溴高锰酸六胺钴(III)的光谱和结构表征
4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230702062b
Berta Barta Holló, Niloofar Bayat, Laura Bereczki, Vladimir Petrusevski, Kende Béres, Attila Farkas, Imre Szilágyi, László Kótai
Structural and spectroscopic characterization (SXRD, IR, liq. N2 temperature Raman, UV) of hexaamminecobalt(III) dibromide permanganate, [Co(NH3)6]Br2(MnO4) (compound 1) are described. There is a 3D hydrogen bond network including N-H???O-Mn and N-H???Br interactions, which could serve as potential reaction centers for solid-phase redox reactions between the ammonia ligands and/or bromide ions as reductants and permanganate ions as oxidant agents. The effect of the nature of halogen ions on the structural and spectroscopic properties of [Co(NH3)6]Br2(MnO4) and the analogous chloride compound, [Co(NH3)6]Cl2(MnO4) (compound 2) are discussed in detail.
介绍了六胺钴(III)二溴高锰酸盐,[Co(NH3)6]Br2(MnO4)(化合物1)的结构和光谱表征(SXRD, IR,液相温度拉曼,UV)。三维氢键网络包括N-H??O-Mn和N-H??Br相互作用,可以作为氨配体和/或溴离子作为还原剂和高锰酸盐离子作为氧化剂之间固相氧化还原反应的潜在反应中心。详细讨论了卤素离子性质对[Co(NH3)6]Br2(MnO4)及其类似氯化合物[Co(NH3)6]Cl2(MnO4)(化合物2)结构和光谱性质的影响。
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引用次数: 0
Health risk assessment of potentially harmful substances from fly ashes generated by coal and coal waste combustion 煤炭和煤矸石燃烧产生的飞灰中潜在有害物质的健康风险评估
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc220130048m
Jovana Buha-Markovic, Ana Marinkovic, J. Savić, Aleksa Krstić, A. Savic, M. Ristić
Lignite and coal waste used as feed fuels in thermal power plants (TPPs) and semi-industrial fluidized bed boiler (FBB), as well as their representative fly ashes (FAs), were examined. Fly ashes were compared employing anions and cations content in correspondent water extracts, trace elements and polycyclic aromatic hydrocarbon concentrations, as well as health risk assessments of substances known to be of concern for public health. Fluoride and sulfate contents in water extracted FAs are far below the legislation limits for waste, classifying all investigated FAs as non-hazardous. Among investigated trace elements, Cd content is the lowest, while Mn content is the highest. The highest enrichment ratios are noticed for As, Pb, Hg, Cu, V and Cr. The results indicate that total PAHs content is elevated in FA from the combustion of coal waste (AFB), with fluoranthene prevailing. The cancer risk of As and the non-cancer risk of As and Ni in some FAs surpass their respective permissible limits. The incremental lifetime cancer risk of an adult population indicates a potential PAHs risk in AFB, whereas all other fly ashes are within safe limits.
对火力发电厂(TPPs)和半工业流化床锅炉(FBB)中作为原料燃料的褐煤和煤矸石及其代表的粉煤灰(FAs)进行了研究。利用相应水提取物中的阴离子和阳离子含量、微量元素和多环芳烃浓度对粉煤灰进行了比较,并对已知对公众健康有影响的物质进行了健康风险评估。水提取的FAs中氟化物和硫酸盐的含量远远低于废物的立法限制,将所有调查的FAs归类为无害。在所研究的微量元素中,Cd含量最低,Mn含量最高。As、Pb、Hg、Cu、V和Cr的富集率最高。结果表明,煤矸石燃烧后的FA中总PAHs含量升高,以氟蒽为主。在一些FAs中,As和Ni的致癌风险和非致癌风险超过了各自的允许限度。成年人群终生癌症风险的增加表明AFB中存在潜在的多环芳烃风险,而所有其他飞灰都在安全范围内。
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引用次数: 0
Physicochemical properties of the heterogeneous system Li2CO3-Na2CO3-K2CO3/MgO Li2CO3-Na2CO3-K2CO3/MgO非均相体系的物理化学性质
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230201023z
I. Zakiryanova, E. Nikolaeva, I. Korzun
The structure, conductivity, melting points and caloric melting effects of the (Li2CO3-Na2CO3-K2CO3)eut melt/MgO nanopowder heterogeneous system with MgO concentration up to 70 vol % have been investigated. A wide variety of methods (DSC, XRD, BET, high resolution scanning electron microscope, AC impedance method, IR and Raman spectroscopy) were used to evaluate samples and research. It is revealed that at the values of effective thickness of the salt phase interlayer between MgO particles below 100 nm there is an abrupt decrease in the melting points of the salt and the normalized phase transition enthalpy of the heterogeneous system. The activation energy of the electrical conductivity rises as the values of effective thickness of the melt phase interlayer between MgO particles decreases. The study established the lack of any chemical interaction between MgO and carbonate melt at 400-600??. In situ Raman spectroscopy of the (Li2CO3-Na2CO3-K2CO3)eut melt/MgO nanopowder systems revealed the solvation of solid particles by salt-melt ions.
研究了MgO浓度高达70 vol %的(Li2CO3-Na2CO3-K2CO3)熔体/MgO纳米粉非均相体系的结构、电导率、熔点和热熔效果。采用多种方法(DSC, XRD, BET,高分辨率扫描电镜,交流阻抗法,IR和拉曼光谱)对样品进行评价和研究。结果表明,当MgO颗粒间盐相层的有效厚度小于100 nm时,盐的熔点和非均相体系的归一化相变焓急剧下降。电导率的活化能随着MgO颗粒间熔相层有效厚度的减小而增大。研究表明,在400 ~ 600℃的温度下,MgO与碳酸盐熔体之间不存在化学相互作用。对(Li2CO3-Na2CO3-K2CO3)熔融体/MgO纳米粉体体系的原位拉曼光谱分析揭示了盐熔离子对固体颗粒的溶剂化作用。
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引用次数: 0
Click mediated synthesis of functionalized glycolipids with peptide-peptoid linkages 点击介导的具有肽-肽-类肽键的功能化糖脂合成
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230201030s
Anadi Singhamahapatra, Chinmayee Pattnaik, Prasad Kar, Chandra Nayak, Narayan Sahoo, Satyanarayan Sahoo
The present work describes the synthesis of a new class of glycolipids with systematic variation in the linkage region as well as in the aglycon part using Cu(I) catalyzed click reaction. The linkage region between sugar and the aglycon part was diversified using amide, amido-triazole, and 5-benzoyl triazole moieties. The structural diversity of glycolipids was further amplified by incorporating several polar peptide foldamer groups such as triazole, amide, peptide, or N-aryl peptoid in the aglycon part of it. The newly designed glycolipids were derived from the amalgamation of different peptide bond mimics. This work reports the first use of N-aryl peptoid in the synthesis of glycolipids. The newly synthesized glycolipids were characterized using different spectroscopic and spectrometric analyses. The impact of the amide bond as well as the triazole ring in the linkage region on the morphology of the glycolipids was analyzed by comparing their self-assembly using SEM analysis. The geometries of the glycolipids were also optimized using density functional theory and the optimized structures were found to be minima in the potential energy surfaces.
本文描述了用Cu(I)催化咔嗒反应合成一类在键区和糖元部分有系统变化的新型糖脂。糖与聚糖部分之间的连接区域由酰胺、氨基三唑和5-苯甲酰三唑组成。糖脂的结构多样性通过在糖基部分加入几个极性肽折叠基团(如三唑、酰胺、肽或n -芳基肽)进一步放大。新设计的糖脂是由不同的肽键模拟物合并而成。本文报道了n -芳基类肽在糖脂合成中的首次应用。用不同的光谱和光谱分析方法对新合成的糖脂进行了表征。利用扫描电镜(SEM)分析了酰胺键和键区三唑环对糖脂形态的影响。利用密度泛函理论对糖脂的几何结构进行了优化,发现优化后的糖脂结构在势能面上最小。
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引用次数: 0
Preventing hydrolysis of AlN powders with organophosphate coating in aqueous media 用有机磷包覆防止AlN粉末在水介质中水解
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230321029k
Ceren Kaya, O. Bayındır, Saruhan Saklar, O. Atakol, Hüseyin Çelikkan
The coating of aluminum nitride (AlN) powder has a great importance industrially and environmentally. AlN can be rapidly hydrolyzed to aluminum hydroxide and ammonia in the atmosphere or water media. To prevent the hydrolysis of AlN, the inorganic or organic based coatings are used frequently. First time, in this study, the phosphate esters as organophosphate coating were used for the inhibition of hydrolysis reaction of AlN in its water suspension. Phenyl phosphate showed the best inhibition against AlN hydrolysis with an easy application technique and as low as 0.005 M diluted concentration. AlN coating efficiency was proved by spectroscopic and imaging methods. It was concluded that the coating acquired the protective properties of phenyl phosphate through its water repellence.
氮化铝粉末涂层具有重要的工业和环境意义。AlN在大气或水介质中可迅速水解为氢氧化铝和氨。为了防止AlN的水解,经常使用无机或有机基涂层。本研究首次采用磷酸酯作为有机磷酸酯包覆物,抑制AlN在水悬浮液中的水解反应。磷酸苯酯对AlN水解的抑制效果最好,应用技术简单,稀释浓度低至0.005 M。通过光谱和成像方法验证了AlN涂层的效率。结果表明,该涂层通过防水性获得了磷酸苯酯的防护性能。
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引用次数: 0
Health risk assessment of toxic elements in sedimentable dust from landfills 垃圾填埋场可沉降粉尘中有毒元素的健康风险评估
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230413032m
U. Marceta, M. Vučinić-Vasić, Jordana Ninkov, Strahinja Ilic, B. Vujic
Four monitoring campaigns of sedimentable dust were provided from two large non-sanitary landfills (Zrenjanin and Novi Sad) in Serbia during 2021. Particle size analysis by laser diffraction and inductively coupled plasma - optical emission spectrometry (ICP-OES) were carried out in order to obtain particle size distribution (PSD) and toxic elements (TEs) concentrations. The health risk assessment of the landfill employees was performed according to United States Environmental Protection Agency (US EPA) methods based on TEs concentrations. The particle size distribution results demonstrated that the majority of sedimentable dust samples mass were not concentrated neither within PM2.5 neither within PM10 fraction. Analysis revealed high concentration of TEs at both landfills: an extremely high concentration of Cr and Zn in samples from Zrenjanin landfill was detected. Health risk potential of elements was as follows for both landfills: Cr > Co > Pb > Ni > Zn > Cu. According to the results, maximal hazard index (HI) for landfill employees in Zrenjanin (1.97*10-1) and Novi Sad (1.13*10-1) showed that non-cancer risk was very low. For both landfill sites, cancer risk (CR) was highest for Cr (2.75*10-5 for Zrenjanin and 2.02*10-7 for Novi Sad), though still within the defined threshold for tolerable cancer risk.
2021年期间,从塞尔维亚的两个大型非卫生垃圾填埋场(Zrenjanin和Novi Sad)开展了四次可沉积粉尘监测活动。采用激光衍射和电感耦合等离子体-光学发射光谱(ICP-OES)分析了样品的粒径分布(PSD)和有毒元素(TEs)浓度。根据美国环境保护署(EPA)基于TEs浓度的方法对垃圾填埋场工作人员进行了健康风险评估。粒径分布结果表明,大部分可沉降尘样品质量既不集中在PM2.5范围内,也不集中在PM10范围内。分析显示,两个垃圾填埋场的TEs浓度都很高:在Zrenjanin垃圾填埋场的样品中检测到极高浓度的Cr和Zn。两个填埋场的元素健康风险潜势如下:Cr > Co > Pb > Ni > Zn > Cu。结果表明,Zrenjanin和Novi Sad的最大危害指数(HI)分别为1.97*10-1和1.13*10-1,非癌风险极低。对于这两个垃圾填埋场,CR的癌症风险(CR)最高(Zrenjanin为2.75*10-5,Novi Sad为2.02*10-7),尽管仍在规定的可耐受癌症风险阈值之内。
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引用次数: 0
Synthetic study on the angular triquinanes 角型三醌类化合物的合成研究
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-01-01 DOI: 10.2298/jsc230627046s
M. Stjepanović, A. Janković, B. Vulovic, R. Matovic, R. Saicic
The synthesis of an angular triquinane, which could serve as a suitable platform for the synthesis of several natural products (panaginsene, silphinene, senoxydene) is described. The synthesis is based on two consecutive cyclopentene annulations, where alkenes were used as latent carbonyl functionalities (via Wacker reaction), and cyclopentenone annulation was effected by aldol condensation.
本文描述了一种角状三醌的合成,它可以作为合成几种天然产物(panaginense, silphinene, senoxydene)的合适平台。该合成基于两个连续环戊烯环,其中烯烃作为潜在羰基官能团(通过瓦克反应),环戊烯酮环是通过醛醇缩合而形成的。
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引用次数: 0
期刊
Journal of The Serbian Chemical Society
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