In this work, a new Organic-Inorganic chloride (H3N–(CH2)6-NH3)[SnCl6] (1) has been synthesized and characterized by single crystal X-ray diffraction (XRD), IR, Raman and impedance spectroscopies. The crystallographic study displays that the title compound crystallizes in the triclinic system with the P−1 space group. The vibrational study (IR, Raman) at room temperature confirmed the existence of the organic and inorganic functional groups. Differential scanning calorimetry (DSC) analysis reveals the existence of three reversible phase transitions at T1 = 345/325 K, T2 = 483/443 K, and T3 = 496/465 K (Heating/Cooling). Furthermore, the conductivity analysis and the dielectric properties confirm the presence of these phase transitions. AC-conductivity measurement of (1) has been investigated using complex impedance spectroscopy in frequency and temperature range 10 Hz–5 MHz and 313–523 K, respectively. The study of Nyquist plots showed the contribution of grains and grain boundaries in the electrical study, confirming the existence of a non-Debye type relaxation. The AC conductivity shows that the material has the potential of impedance sensors.
本研究合成了一种新的有机无机氯化物（H3N-(CH2)6-NH3）[SnCl6] (1)，并通过单晶 X 射线衍射 (XRD)、红外光谱、拉曼光谱和阻抗光谱对其进行了表征。晶体学研究表明，标题化合物在 P-1 空间群的三菱系中结晶。室温下的振动研究（红外光谱、拉曼光谱）证实了有机和无机官能团的存在。差示扫描量热法（DSC）分析表明，在 T1 = 345/325 K、T2 = 483/443 K 和 T3 = 496/465 K（加热/冷却）存在三个可逆相变。此外，电导率分析和介电特性也证实了这些相变的存在。在频率和温度范围分别为 10 Hz-5 MHz 和 313-523 K 时，使用复阻抗光谱对 (1) 的交流电导率测量进行了研究。奈奎斯特图的研究表明，晶粒和晶界在电学研究中的作用，证实了非戴贝型弛豫的存在。交流电导率表明该材料具有阻抗传感器的潜力。
{"title":"A new organic–inorganic chloride (H3N–(CH2)6–NH3)[SnCl6]: Crystal structure, thermal analysis, vibrational study, and electrical properties","authors":"Hannachi Nejeh , Abderrazek Oueslati , Walid Rekik","doi":"10.1016/j.poly.2024.117250","DOIUrl":"10.1016/j.poly.2024.117250","url":null,"abstract":"<div><div>In this work, a new Organic-Inorganic chloride (H<sub>3</sub>N–(CH<sub>2</sub>)<sub>6</sub>-NH<sub>3</sub>)[SnCl<sub>6</sub>] (<strong>1</strong>) has been synthesized and characterized by single crystal X-ray diffraction (XRD), IR, Raman and impedance spectroscopies. The crystallographic study displays that the title compound crystallizes in the triclinic system with the <em>P</em>−1 space group. The vibrational study (IR, Raman) at room temperature confirmed the existence of the organic and inorganic functional groups. Differential scanning calorimetry (DSC) analysis reveals the existence of three reversible phase transitions at T<sub>1</sub> = 345/325 K, T<sub>2</sub> = 483/443 K, and T<sub>3</sub> = 496/465 K (Heating/Cooling). Furthermore, the conductivity analysis and the dielectric properties confirm the presence of these phase transitions. AC-conductivity measurement of (<strong>1</strong>) has been investigated using complex impedance spectroscopy in frequency and temperature range 10 Hz–5 MHz and 313–523 K, respectively. The study of Nyquist plots showed the contribution of grains and grain boundaries in the electrical study, confirming the existence of a non-Debye type relaxation. The AC conductivity shows that the material has the potential of impedance sensors.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117250"},"PeriodicalIF":2.4,"publicationDate":"2024-10-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142441400","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-10DOI: 10.1016/j.poly.2024.117254
Sana Ghaffar , Adeel Ahmed , Muhammad Jamshaid , Wedad A. Al-onazi , M. Ajmal Ali , Amjad Iqbal , Rashid Iqbal
This research aims to develop the highly promising Fe2O3/g-C3N4 photocatalyst through hydrothermal techniques to cope with the elevated amounts of bromophenol blue (BPB) dye in wastewater. The morphological studies were carried out by SEM analysis, while the crystallinity, structural behavior, and oxidation states of the prepared materials were determined by XRD, FTIR, and XPS analysis. The hydrodynamic size, surface area, and magnetic characteristics of the constructed materials were assessed through DLS, BET, and VSM analysis. The effectivity of the synthesized Fe2O3 and Fe2O3/g-C3N4-30 photocatalysts was appraised by the abatement of BPB under visible light radiation for 48 min. The results have shown an excellent degradation efficacy of Fe2O3/g-C3N4-30 photocatalyst with 98.39 % of BPB removal and a rate constant of 0.0757 min−1, which was much higher than Fe2O3 photocatalyst with 79.64 % of removal and a rate constant of 0.0335 min−1 under optimum conditions. The enhancement in degradation efficiency of the Fe2O3/g-C3N4-30 was due to the large surface area of Fe2O3/g-C3N4-30 (106.94 m2/g) as a result of g-C3N4 inclusion in the material, while the pure Fe2O3 unveiled a surface area of 89.67 m2/g. The impact of different reaction parameters on BPB degradation was also investigated, while the contribution of free radicals was corroborated through radical trapping experiments. The Fe2O3/g-C3N4-30 exhibited tremendous stability for repeated applications, with a loss of 8.03 % in efficiency after five consecutive experiments because of its easy magnetic separation. The experimental results have shown that synthesized Fe2O3/g-C3N4-30 photocatalysts could be used for the effective degradation of BPB from wastewater.
{"title":"Construction of visible-light-induced Fe2O3/g-C3N4 nanocomposites for the enhanced degradation of organic dyes: Optimization of operative parameters","authors":"Sana Ghaffar , Adeel Ahmed , Muhammad Jamshaid , Wedad A. Al-onazi , M. Ajmal Ali , Amjad Iqbal , Rashid Iqbal","doi":"10.1016/j.poly.2024.117254","DOIUrl":"10.1016/j.poly.2024.117254","url":null,"abstract":"<div><div>This research aims to develop the highly promising Fe<sub>2</sub>O<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub> photocatalyst through hydrothermal techniques to cope with the elevated amounts of bromophenol blue (BPB) dye in wastewater. The morphological studies were carried out by SEM analysis, while the crystallinity, structural behavior, and oxidation states of the prepared materials were determined by XRD, FTIR, and XPS analysis. The hydrodynamic size, surface area, and magnetic characteristics of the constructed materials were assessed through DLS, BET, and VSM analysis. The effectivity of the synthesized Fe<sub>2</sub>O<sub>3</sub> and Fe<sub>2</sub>O<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub>-30 photocatalysts was appraised by the abatement of BPB under visible light radiation for 48 min. The results have shown an excellent degradation efficacy of Fe<sub>2</sub>O<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub>-30 photocatalyst with 98.39 % of BPB removal and a rate constant of 0.0757 min<sup>−1</sup>, which was much higher than Fe<sub>2</sub>O<sub>3</sub> photocatalyst with 79.64 % of removal and a rate constant of 0.0335 min<sup>−1</sup> under optimum conditions. The enhancement in degradation efficiency of the Fe<sub>2</sub>O<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub>-30 was due to the large surface area of Fe<sub>2</sub>O<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub>-30 (106.94 m<sup>2</sup>/g) as a result of g-C<sub>3</sub>N<sub>4</sub> inclusion in the material, while the pure Fe<sub>2</sub>O<sub>3</sub> unveiled a surface area of 89.67 m<sup>2</sup>/g. The impact of different reaction parameters on BPB degradation was also investigated, while the contribution of free radicals was corroborated through radical trapping experiments. The Fe<sub>2</sub>O<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub>-30 exhibited tremendous stability for repeated applications, with a loss of 8.03 % in efficiency after five consecutive experiments because of its easy magnetic separation. The experimental results have shown that synthesized Fe<sub>2</sub>O<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub>-30 photocatalysts could be used for the effective degradation of BPB from wastewater.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117254"},"PeriodicalIF":2.4,"publicationDate":"2024-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142437659","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-10DOI: 10.1016/j.poly.2024.117253
Mohd Mustafa , Tabee Jan , Shabnam Raheem , Junaid Afzal , Naveed Nazir , Mubashir Hussain Masoodi , Masood Ahmad Rizvi
Decorating chemical motifs with appropriate functional groups capable of supramolecular interactions hold key in modulating these novel systems for targeted applications. This work by means of a comparative study of Ferrocene and Ferrocenyl α- aminophosphonate highlight supradecoration induced multi paradigm properties across materials to medicine. The observed results indicate an increase in crystal framework energy with induction of mechanochromism and aggregation-induced emission in case of Ferrocenyl-α-amino phosphonate as novel supra decorated Ferrocene motif. Comparative BSA and BLC studies indicated improved biocompatibility with enhancement of catalase enzyme activity in case of Ferrocenyl-α- aminophosphonate compared to pristine Ferrocene. The relative quantification of intermolecular non covalent interactions of Ferrocene and Ferrocenyl-α- aminophosphonate evaluated using Quantum crystallographic methods and non-covalent interaction analysis were used to corroborate the supramodulation effects. The observed influence of Ferrocenyl α-aminophosphonate on the enzymatic activity of catalase was also examined using a comparative molecular docking analysis. The docking results corroborated influence of supradecoration on binding affinity and binding site, which are vital for designing ligands of enhanced catalase activity and also helpful in prediction of newer regulatory sites on enzyme. Taken together this work signifies how supra decoration of Ferrocene motif with functionalities capable of diverse intermolecular non-covalent interactions modulate molecular properties for newer applications.
{"title":"Supradecoration induced novel Properties: A comparative study of Ferrocene and Ferrocenyl α-aminophosphonate","authors":"Mohd Mustafa , Tabee Jan , Shabnam Raheem , Junaid Afzal , Naveed Nazir , Mubashir Hussain Masoodi , Masood Ahmad Rizvi","doi":"10.1016/j.poly.2024.117253","DOIUrl":"10.1016/j.poly.2024.117253","url":null,"abstract":"<div><div>Decorating chemical motifs with appropriate functional groups capable of supramolecular interactions hold key in modulating these novel systems for targeted applications. This work by means of a comparative study of Ferrocene and Ferrocenyl α- aminophosphonate highlight supradecoration induced multi paradigm properties across materials to medicine. The observed results indicate an increase in crystal framework energy with induction of mechanochromism and aggregation-induced emission in case of Ferrocenyl-α-amino phosphonate as novel supra decorated Ferrocene motif. Comparative BSA and BLC studies indicated improved biocompatibility with enhancement of catalase enzyme activity in case of Ferrocenyl-α- aminophosphonate compared to pristine Ferrocene. The relative quantification of intermolecular non covalent interactions of Ferrocene and Ferrocenyl-α- aminophosphonate evaluated using Quantum crystallographic methods and non-covalent interaction analysis were used to corroborate the supramodulation effects. The observed influence of Ferrocenyl α-aminophosphonate on the enzymatic activity of catalase was also examined using a comparative molecular docking analysis. The docking results corroborated influence of supradecoration on binding affinity and binding site, which are vital for designing ligands of enhanced catalase activity and also helpful in prediction of newer regulatory sites on enzyme. Taken together this work signifies how supra decoration of Ferrocene motif with functionalities capable of diverse intermolecular non-covalent interactions modulate molecular properties for newer applications.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117253"},"PeriodicalIF":2.4,"publicationDate":"2024-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142441401","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
In recent years, the employment of transition metal complexes for working electrode surface modification for sensor fabrication has become an area of research direction. Based on this, in this study, three Co(II) complexes: Co(phen)Cl2 (CoC12H8N2Cl2) (C1), and Brønsted–Lowry acids Co(phen)(HTA)Cl (CoC16H13N2O6Cl)(C2), and Co(phen)(HTA)2 (CoC20H18N2O12)(C3) were synthesized and characterized using various techniques such as UV–Vis, FT-IR, ICP OES, TGA, DTA, pXRD as well as electrolytic conductivity, and acid-base property analysis. C and C3 were found polycrystalline whose size falls within the nano range of 50 and 51 nm, respectively. The synthesis was intended to get materials for voltammetrically modifying glassy carbon electrodes for the determination of salbutamol. Salbutamol is a short-acting β2 adrenergic receptor agonist that is applied for opening the medium and large airways in the lungs and eventually treats asthma among other problems. The electrochemical application of the synthesized materials was studied by fabricating through electropolymerization of C1, C2, and C3 on glassy carbon electrodes. The poly(C1)/GCE, poly(C2)/GCE, and poly(C3)/GCE) revealed effective surface area is 0.174 cm2, 0.183 cm2, and 0.281 cm2, respectively, and electrochemical catalysis of the materials increased with the number of the tartrate. The Rct values are 5686, 242, 216, and 185 Ω cm2, while the Cdl values are 9.93 × 10−8, 5.35 × 10−6, 1.25 × 10−5, and 2.72 × 10−5, for bare GCE, poly(C1)/GCE, poly(C2)/GCE and poly(C3)/GCE, respectively. Similarly, the rate of charge transfer (k°) increased significantly on the modified electrode compared to the bare GCE. Salbutamol demonstrated a single well-shaped irreversible oxidative peak at the modified electrodes in the ascending order of poly(C1)/GCE, poly(C2)/GCE, and poly(C3)/GCE when compared to a bare GCE.
{"title":"New Brønsted–Lowry acid Co(II) complexes: Synthesis, characterization, and investigation of electrochemical application for sensing of salbutamol","authors":"Bosena Dinber , Kidanemariam Teklay Hilawea , Endalamaw Yihune , Getasil Chanie , Melaku Metto , Mamaru Bitew , Getinet Tamiru Tigineh , Atakilt Abebe","doi":"10.1016/j.poly.2024.117248","DOIUrl":"10.1016/j.poly.2024.117248","url":null,"abstract":"<div><div>In recent years, the employment of transition metal complexes for working electrode surface modification for sensor fabrication has become an area of research direction. Based on this, in this study, three Co(II) complexes: Co(phen)Cl<sub>2</sub> (CoC<sub>12</sub>H<sub>8</sub>N<sub>2</sub>Cl<sub>2</sub>) (<strong>C1</strong>), and <strong>Brønsted–Lowry acids</strong> Co(phen)(HTA)Cl (CoC<sub>16</sub>H<sub>13</sub>N<sub>2</sub>O<sub>6</sub>Cl)(<strong>C2</strong>), and Co(phen)(HTA)<sub>2</sub> (CoC<sub>20</sub>H<sub>18</sub>N<sub>2</sub>O<sub>12</sub>)(<strong>C3</strong>) were synthesized and characterized using various techniques such as UV–Vis, FT-IR, ICP OES, TGA, DTA, pXRD as well as electrolytic conductivity, and acid-base property analysis. C and C3 were found polycrystalline whose size falls within the nano range of 50 and 51 nm, respectively. The synthesis was intended to get materials for voltammetrically modifying glassy carbon electrodes for the determination of salbutamol. Salbutamol<!--> <!-->is a short-acting β<sub>2</sub> <!-->adrenergic receptor agonist that is applied for opening the medium and large airways in the lungs and eventually treats asthma among other problems. The electrochemical application of the synthesized materials was studied by fabricating through electropolymerization of C1, C2, and C3 on glassy carbon electrodes. The poly(C1)/GCE, poly(C2)/GCE, and poly(C3)/GCE) revealed effective surface area is 0.174 cm<sup>2</sup>, 0.183 cm<sup>2</sup>, and 0.281 cm<sup>2</sup>, respectively, and electrochemical catalysis of the materials increased with the number of the tartrate. The Rct values are 5686, 242, 216, and 185 Ω cm<sup>2</sup>, while the C<sub>dl</sub> values are 9.93 × 10<sup>−8</sup>, 5.35 × 10<sup>−6</sup>, 1.25 × 10<sup>−5</sup>, and 2.72 × 10<sup>−5</sup>, for bare GCE, poly(C1)/GCE, poly(C2)/GCE and poly(C3)/GCE, respectively. Similarly, the rate of charge transfer (k°) increased significantly on the modified electrode compared to the bare GCE. Salbutamol demonstrated a single well-shaped irreversible oxidative peak at the modified electrodes in the ascending order of poly(C1)/GCE, poly(C2)/GCE, and poly(C3)/GCE when compared to a bare GCE.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117248"},"PeriodicalIF":2.4,"publicationDate":"2024-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142416251","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-10DOI: 10.1016/j.poly.2024.117249
Nikolay A. Bumagin , Irina A. Kolesnik , Vladimir I. Potkin , Evgeniy A. Dikusar , Alexander S. Lyakhov , Ludmila S. Ivashkevich , Hongwei Zhou , Wenliang Li
Synthesis, characterization, and catalytic activity of palladium(II) complexes containing tridentate N-(pyridin-2-yl)-1,2-azol-3-carboxamide ligands with various length amide linkers [CONH(CH2)n, n = 0,1,2] is reported. Complexation of previously undescribed mixed pyridin-azol-carboxamide ligands with PdCl2 occurs unusually by deprotonation of the amide group and elimination of HCl affording the palladium(II) pincer complexes [(k3-NNN)PdCl]n (n = 1, 2), which was proven by single crystal X-ray diffraction. The first time synthesized complexes are high-turnover catalysts, as was shown during the evaluation in Suzuki reaction between aryl halides and arylboronic acids: substituted biaryls, including practically significant, were obtained with up to quantitative yields under Green Chemistry conditions.
报告了含有三叉 N-(吡啶-2-基)-1,2-氮唑-3-甲酰胺配体和不同长度酰胺连接体 [CONH(CH2)n, n = 0,1,2] 的钯（II）配合物的合成、表征和催化活性。以前未曾描述过的吡啶-偶氮唑-3-甲酰胺混合配体与 PdCl2 的络合异常地通过酰胺基团的去质子化和 HCl 的消除而发生，从而得到钯（II）钳形配合物 [(k3-NNN)PdCl]n (n = 1, 2)，单晶 X 射线衍射证明了这一点。在芳基卤化物和芳基硼酸的铃木反应中进行的评估表明，首次合成的配合物是一种高转化率催化剂：在绿色化学条件下，得到的取代双芳基（包括实际上重要的取代双芳基）的产率高达定量。
{"title":"Palladium(II) complexes of N-(pyridin-2-yl)-1,2-azol-3-carboxamide derived NNN-pincer ligands: Synthesis, unusual complexation and high-turnover catalysis in water","authors":"Nikolay A. Bumagin , Irina A. Kolesnik , Vladimir I. Potkin , Evgeniy A. Dikusar , Alexander S. Lyakhov , Ludmila S. Ivashkevich , Hongwei Zhou , Wenliang Li","doi":"10.1016/j.poly.2024.117249","DOIUrl":"10.1016/j.poly.2024.117249","url":null,"abstract":"<div><div>Synthesis, characterization, and catalytic activity of palladium(II) complexes containing tridentate <em>N</em>-(pyridin-2-yl)-1,2-azol-3-carboxamide ligands with various length amide linkers [CONH(CH<sub>2</sub>)<em><sub>n</sub></em>, <em>n</em> = 0,1,2] is reported. Complexation of previously undescribed mixed pyridin-azol-carboxamide ligands with PdCl<sub>2</sub> occurs unusually by deprotonation of the amide group and elimination of HCl affording the palladium(II) pincer complexes [(k<sup>3</sup>-NNN)PdCl]<em><sub>n</sub></em> (<em>n</em> = 1, 2), which was proven by single crystal X-ray diffraction. The first time synthesized complexes are high-turnover catalysts, as was shown during the evaluation in Suzuki reaction between aryl halides and arylboronic acids: substituted biaryls, including practically significant, were obtained with up to quantitative yields under Green Chemistry conditions.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117249"},"PeriodicalIF":2.4,"publicationDate":"2024-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142441402","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
This study reported the synthesis of two new ligands (1,2) and their Ru(II)-enaminone complexes (3,4). The Ru(II) complexes were obtained from the reaction of the [RuCl2(p-cymene)]2 dimers with the new enaminone derivative ligands (1,2). The use of standard spectroscopy techniques entirely characterized the compounds. Single crystal studies investigated the crystal structure of ligand (1) and complexes (3,4). X-ray diffraction data analysis was used to confirm the enaminone form of 1. Also, 3 and 4 exhibited the classical three-legged piano stool structure with Ru(II) coordinated by the nitrogen and oxygen atoms of 1 and a chloride ligand as the legs and the η6-π-bound p-cymene ligand occupies the seat of the piano stool. The Ru(II) complexes have been studied as catalysts in the transfer hydrogenation of acetophenone and other various ketones in the presence of KOtBu. The catalytic conditions were optimized using different substrate/catalyst and base/catalyst ratios. We found that the complexes show good activities and up to 100 % selectivity. The best turnover frequency (1667 h−1) was found for 3 when using acetophenone as the substrate.
{"title":"Application of enaminone ruthenium(II) complexes as catalysts in the transfer hydrogenation of ketones","authors":"Rukiye Fırıncı , Erkan Fırıncı , Resul Sevinçek , Muhittin Aygün","doi":"10.1016/j.poly.2024.117247","DOIUrl":"10.1016/j.poly.2024.117247","url":null,"abstract":"<div><div>This study reported the synthesis of two new ligands (<strong>1</strong>,<strong>2</strong>) and their Ru(II)-enaminone complexes (<strong>3</strong>,<strong>4</strong>). The Ru(II) complexes were obtained from the reaction of the [RuCl<sub>2</sub>(p-cymene)]<sub>2</sub> dimers with the new enaminone derivative ligands (<strong>1</strong>,<strong>2</strong>). The use of standard spectroscopy techniques entirely characterized the compounds. Single crystal studies investigated the crystal structure of ligand (<strong>1</strong>) and complexes (<strong>3</strong>,<strong>4</strong>). X-ray diffraction data analysis was used to confirm the enaminone form of <strong>1</strong>. Also, <strong>3</strong> and <strong>4</strong> exhibited the classical three-legged piano stool structure with Ru(II) coordinated by the nitrogen and oxygen atoms of <strong>1</strong> and a chloride ligand as the legs and the η<sup>6</sup>-π-bound p-cymene ligand occupies the seat of the piano stool. The Ru(II) complexes have been studied as catalysts in the transfer hydrogenation of acetophenone and other various ketones in the presence of KO<em><sup>t</sup></em>Bu. The catalytic conditions were optimized using different substrate/catalyst and base/catalyst ratios. We found that the complexes show good activities and up to 100 % selectivity. The best turnover frequency (1667 h<sup>−1</sup>) was found for <strong>3</strong> when using acetophenone as the substrate.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117247"},"PeriodicalIF":2.4,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142437527","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
In this study, 4,5-dicyano-1,2-phenylene dinicotinate compound was obtained as a result of the reaction of 4,5-dichlorophthalonitrile and nicotinic acid. This compound was reacted with the zinc chloride salt to obtain the original zinc phthalocyanine compound bearing 1,2-phenylene bis(3-chloropropanoate) substituted groups. This compound and its starting material were characterized with the assist of 1H NMR, IR, UV–vis, Mass spectrum. In the docking study of compounds (3) and (4) against each target (AChE, BChE, α-Amy and α-Gly), Zn complex (4) exhibits more binding affinity with the target models considered compared to ligand structure (3). Especially, AChE protein and complex (4) form the best binding affinity with a binding energy value of −10.55 kcal/mol. They are compatible and supportive with the data obtained as a result of in vitro analysis. These 4,5-dicyano-1,2-phenylene dinicotinate (3) and 2, 10, 16, 24 – tetrakis 1,2-phenylene bis(3-chloropropanoate) phthalocyaninato) zinc(II) (4) complexes had effective inhibition against α-glucosidase, α-amylase, butyrylcholinesterase and AChE. Also, IC50 amounts were found as 7.84 and 12.36 µM for AChE, 3.80 and 4.56 µM for BChE, 27.08 and 38.14 µM for α-amylase, and 5.30 and 9.73 µM for α-glucosidase.
{"title":"Synthesis of zinc phthalocyanine containing 1,2-phenylene bis(3-chloropropanoate) substituted groups and investigation of their metabolic enzyme inhibitory effects","authors":"Derya Güngördü Solğun , Nastaran Sadeghian , Parham Taslimi , Tugba Taskin-Tok , Mehmet Salih Ağırtaş","doi":"10.1016/j.poly.2024.117251","DOIUrl":"10.1016/j.poly.2024.117251","url":null,"abstract":"<div><div>In this study, 4,5-dicyano-1,2-phenylene dinicotinate compound was obtained as a result of the reaction of 4,5-dichlorophthalonitrile and nicotinic acid. This compound was reacted with the zinc chloride salt to obtain the original zinc phthalocyanine compound bearing 1,2-phenylene bis(3-chloropropanoate) substituted groups. This compound and its starting material were characterized with the assist of <sup>1</sup>H NMR, IR, UV–vis, Mass spectrum. In the docking study of compounds (<strong>3</strong>) and (<strong>4</strong>) against each target (AChE, BChE, α-Amy and α-Gly), Zn complex (<strong>4</strong>) exhibits more binding affinity with the target models considered compared to ligand structure (<strong>3</strong>). Especially, AChE protein and complex (<strong>4</strong>) form the best binding affinity with a binding energy value of −10.55 kcal/mol. They are compatible and supportive with the data obtained as a result of in vitro analysis. These 4,5-dicyano-1,2-phenylene dinicotinate (<strong>3</strong>) and 2, 10, 16, 24 – tetrakis 1,2-phenylene bis(3-chloropropanoate) phthalocyaninato) zinc(II) (<strong>4</strong>) complexes had effective inhibition against α-glucosidase, α-amylase, butyrylcholinesterase and AChE. Also, IC<sub>50</sub> amounts were found as 7.84 and 12.36 µM for AChE, 3.80 and 4.56 µM for BChE, 27.08 and 38.14 µM for α-amylase, and 5.30 and 9.73 µM for α-glucosidase.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117251"},"PeriodicalIF":2.4,"publicationDate":"2024-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142437528","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The reaction of PdCl2 and Pd(OAc)2 with (E)-2-(2-(pyridin-2-ylmethylene)hydrazinyl)benzo[d]thiazole (HL) in methanol resulted in the formation of two neutral mononuclear Pd(II) complexes. By using PdCl2 two kinds of crystals with general formula of [Pd(Cl)L]·0.5(C2H5OH) (1a) and [Pd(Cl)L] (1b) were obtained while Pd(OAc)2 gave one type of crystal with general formula of [Pd(OAc)L]·0.5(H2O) (2). These complexes were characterized using spectroscopic methods, and their molecular structures were determined by single crystal X-ray diffraction analysis. In these complexes, the ligand coordinates to the Pd(II) core through the nitrogen atoms of the thiazole ring, pyridine ring, and imine moiety, acting as tridentate mononegative NNN donor ligand. These palladium(II) complexes were also found to exhibit catalytic activity in Suzuki-Miyaura coupling reactions.
{"title":"Palladium(II) complexes comprising thiazole-hydrazone Schiff base ligand: Synthesis, structure and catalytic activity in Suzuki-Miyaura coupling reactions","authors":"Zahra Bagheri , Massomeh Ghorbanloo , Rahman Bikas , Tadeusz Lis","doi":"10.1016/j.poly.2024.117245","DOIUrl":"10.1016/j.poly.2024.117245","url":null,"abstract":"<div><div>The reaction of PdCl<sub>2</sub> and Pd(OAc)<sub>2</sub> with (<em>E</em>)-2-(2-(pyridin-2-ylmethylene)hydrazinyl)benzo[<em>d</em>]thiazole (<strong>HL</strong>) in methanol resulted in the formation of two neutral mononuclear Pd(II) complexes. By using PdCl<sub>2</sub> two kinds of crystals with general formula of [Pd(Cl)L]·0.5(C<sub>2</sub>H<sub>5</sub>OH) (<strong>1a</strong>) and [Pd(Cl)L] (<strong>1b</strong>) were obtained while Pd(OAc)<sub>2</sub> gave one type of crystal with general formula of [Pd(OAc)L]·0.5(H<sub>2</sub>O) (<strong>2</strong>). These complexes were characterized using spectroscopic methods, and their molecular structures were determined by single crystal X-ray diffraction analysis. In these complexes, the ligand coordinates to the Pd(II) core through the nitrogen atoms of the thiazole ring, pyridine ring, and imine moiety, acting as tridentate mononegative NNN donor ligand. These palladium(II) complexes were also found to exhibit catalytic activity in Suzuki-Miyaura coupling reactions.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117245"},"PeriodicalIF":2.4,"publicationDate":"2024-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142416252","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-03DOI: 10.1016/j.poly.2024.117242
Mukesh Kawad , Sagar Sangani , Jigneshkumar Parmar , Ranjitsinh C. Dabhi , Prashant S. Arya , Nishith Teraiya , Sarfaraz Ahmed , Rakesh Kumar Ameta
An organometallic series based on 2-ferrocene-4-amine-1H-benzo[d]imidazole derivative has been synthesized and characterized through FTIR, H/CNMR, and LCMS. Their antimicrobial activity was assessed by testing them against B. subtills, Staphylococcus aureus, E. faecalis, S. marcescens, E. coli, K. pneumoniae, C. albicans, A. niger, Mucor sp. where they showed good zone of inhibition (ZOI) as compared to standards. The cytotoxicity of synthesized compounds was tested against Hela (cervical) and MCF-7 (breast) cancer cell lines where compound 5a and 5b displayed equivalent potency to the standard while 5e demonstrated highest cytotoxicity against both cell lines. Their comparative docking analysis with DNA suggested that docking score of 5e was −7.4 kcal/mol versus −6 kcal/mol of ethidium bromide, indicating that our designed compound acts via DNA intercalation.
我们合成了一个基于 2-二茂铁-4-胺-1H-苯并[d]咪唑衍生物的有机金属系列，并通过傅立叶变换红外光谱、H/CNMR 和 LCMS 对其进行了表征。通过测试这些衍生物对枯草杆菌、金黄色葡萄球菌、粪大肠杆菌、肉毒杆菌、大肠杆菌、肺炎双球菌、白僵菌、黑僵菌、粘孢子菌的抗菌活性，与标准物质相比，这些衍生物显示出良好的抑制区（ZOI）。合成的化合物对 Hela（宫颈癌）和 MCF-7（乳腺癌）细胞系进行了细胞毒性测试，结果表明化合物 5a 和 5b 与标准化合物的效力相当，而 5e 对这两种细胞系的细胞毒性最高。他们与 DNA 的对比对接分析表明，5e 的对接得分为 -7.4 kcal/mol，而溴化乙锭的对接得分为 -6 kcal/mol，这表明我们设计的化合物通过 DNA 插层发挥作用。
{"title":"2-Ferrocene-4-amine-1H-benzo[d]imidazole and their derivatives: Synthesis, biological and docking study","authors":"Mukesh Kawad , Sagar Sangani , Jigneshkumar Parmar , Ranjitsinh C. Dabhi , Prashant S. Arya , Nishith Teraiya , Sarfaraz Ahmed , Rakesh Kumar Ameta","doi":"10.1016/j.poly.2024.117242","DOIUrl":"10.1016/j.poly.2024.117242","url":null,"abstract":"<div><div>An organometallic series based on 2-ferrocene-4-amine-1<em>H</em>-benzo[<em>d</em>]imidazole derivative has been synthesized and characterized through FTIR, <sup>H/C</sup>NMR, and LCMS. Their antimicrobial activity was assessed by testing them against <em>B. subtills</em>, Staphylococcus aureus, <em>E. faecalis, S. marcescens, E. coli, K. pneumoniae, C. albicans, A. niger, Mucor sp</em>. where they showed good zone of inhibition (ZOI) as compared to standards. The cytotoxicity of synthesized compounds was tested against Hela (cervical) and MCF-7 (breast) cancer cell lines where compound 5a and 5b displayed equivalent potency to the standard while 5e demonstrated highest cytotoxicity against both cell lines. Their comparative docking analysis with DNA suggested that docking score of <strong>5e</strong> was −7.4 kcal/mol versus −6 kcal/mol of ethidium bromide, indicating that our designed compound acts <em>via</em> DNA intercalation.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117242"},"PeriodicalIF":2.4,"publicationDate":"2024-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142416253","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-03DOI: 10.1016/j.poly.2024.117246
Xiaojing Mao , Huachang Li , Yehong Shi , Jiemin Liu , Lijun Kuai , Fei Yang , Chenmin Wu
Recognition and detection of Fe3+ and Al3+ ions in water are important for human health and life. Herein, a novel multifunctional fluorescence sensor based on zinc-based metal-organic frameworks (Zn-MOF) was developed using zinc nitrate hexahydrate and pyridine-2,5-dicarboxylic acid by solvothermal condition, and characterized by X-ray single crystal diffraction, elemental analysis, powder X-ray diffraction (PXRD), etc. The PXRD experiment results observed that the structure of Zn-MOF is rearranged after water molecules exchanged all 3 DMF solvates in the pores. Fluorescent sensing experiments revealed that Zn-MOF exhibits high sensitivity in detecting Fe3+ and Al3+ by significant fluorescence quenching. The limit of detection (LOD) of Fe3+ and Al3+ were 0.18 μM and 0.064 μM, respectively. The anti-interference experiment revealing that Zn-MOF has a high selectivity to detect Fe3+ and Al3+. In addition, the quenching mechanism of Zn-MOF was demonstrated to be attributed to the inner filter effect (IFE). Furthermore, in the real sample detection of tap water, the recoveries of Fe3+ and Al3+ were 103.0 %–107.9 % and 106.1 %–110.5 %, respectively, and the relative standard deviations (RSD) were less than 7.42 % and 6.20 %, respectively. This work provided an reliable method for the quantitative detection of Fe3+ and Al3+ and was successfully applied in tap water with satisfactory recovery and precision.
{"title":"A multifunctional fluorescence sensor based Zn(II) metal-organic framework for rapid and sensitive detection Fe3+ and Al3+","authors":"Xiaojing Mao , Huachang Li , Yehong Shi , Jiemin Liu , Lijun Kuai , Fei Yang , Chenmin Wu","doi":"10.1016/j.poly.2024.117246","DOIUrl":"10.1016/j.poly.2024.117246","url":null,"abstract":"<div><div>Recognition and detection of Fe<sup>3+</sup> and Al<sup>3+</sup> ions in water are important for human health and life. Herein, a novel multifunctional fluorescence sensor based on zinc-based metal-organic frameworks (Zn-MOF) was developed using zinc nitrate hexahydrate and pyridine-2,5-dicarboxylic acid by solvothermal condition, and characterized by X-ray single crystal diffraction, elemental analysis, powder X-ray diffraction (PXRD), etc. The PXRD experiment results observed that the structure of Zn-MOF is rearranged after water molecules exchanged all 3 DMF solvates in the pores. Fluorescent sensing experiments revealed that Zn-MOF exhibits high sensitivity in detecting Fe<sup>3+</sup> and Al<sup>3+</sup> by significant fluorescence quenching. The limit of detection (LOD) of Fe<sup>3+</sup> and Al<sup>3+</sup> were 0.18 μM and 0.064 μM, respectively. The anti-interference experiment revealing that Zn-MOF has a high selectivity to detect Fe<sup>3+</sup> and Al<sup>3+</sup>. In addition, the quenching mechanism of Zn-MOF was demonstrated to be attributed to the inner filter effect (IFE). Furthermore, in the real sample detection of tap water, the recoveries of Fe<sup>3+</sup> and Al<sup>3+</sup> were 103.0 %–107.9 % and 106.1 %–110.5 %, respectively, and the relative standard deviations (RSD) were less than 7.42 % and 6.20 %, respectively. This work provided an reliable method for the quantitative detection of Fe<sup>3+</sup> and Al<sup>3+</sup> and was successfully applied in tap water with satisfactory recovery and precision.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117246"},"PeriodicalIF":2.4,"publicationDate":"2024-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142416250","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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