Two new heteronuclear Cd(II)/Pd(II) coordination polymers, [Cd2(µ-im)2(Him)4Pd(µ-CN)4]n (1) and [Cd(Him)2Pd(µ-CN)4]n (2) (Him: imidazole), have been synthesized under different conditions and characterized using elemental analysis, thermal analysis, FT-IR and Raman spectroscopy, single-crystal and powder X-ray diffraction techniques. In 1, the Cd(II) ions are bridged by imidazolate ligands to generate 1D chain structure. Neighbouring 1D chains were linked by [Pd(CN)4]2- ions to form 3D framework. In 2, the metal ions are bridged by cyanide ligands to generate 2D [Cd2Pd2(µ-CN)4]n network. Catalytic peroxidative oxidation activity of 1 and 2 was examined on the oxidation of benzyl alcohol using tertiary-butyl hydroperoxide (t-BuOOH) as the oxygen source. The compound 1 exhibited over 90 % product conversion at 80 °C in 24-hour reaction time. In addition, the catalyst exhibited high selectivity towards benzaldehyde and no over-oxidation product (benzoic acid) was detected.
{"title":"Heteronuclear coordination polymers with imidazole ligand: Synthesis, characterization and alcohol oxidation activities","authors":"Güneş Süheyla Kürkçüoğlu , Okan Zafer Yeşilel , Telvin Mwanza , Seray Kekeç , Hakan Ünver , Onur Şahin","doi":"10.1016/j.poly.2024.117263","DOIUrl":"10.1016/j.poly.2024.117263","url":null,"abstract":"<div><div>Two new heteronuclear Cd(II)/Pd(II) coordination polymers, [Cd<sub>2</sub>(µ-im)<sub>2</sub>(Him)<sub>4</sub>Pd(µ-CN)<sub>4</sub>]<sub>n</sub> (<strong>1</strong>) and [Cd(Him)<sub>2</sub>Pd(µ-CN)<sub>4</sub>]<sub>n</sub> (<strong>2</strong>) (Him: imidazole), have been synthesized under different conditions and characterized using elemental analysis, thermal analysis, FT-IR and Raman spectroscopy, single-crystal and powder X-ray diffraction techniques. In <strong>1</strong>, the Cd(II) ions are bridged by imidazolate ligands to generate 1D chain structure. Neighbouring 1D chains were linked by [Pd(CN)<sub>4</sub>]<sup>2-</sup> ions to form 3D framework. In <strong>2</strong>, the metal ions are bridged by cyanide ligands to generate 2D [Cd<sub>2</sub>Pd<sub>2</sub>(µ-CN)<sub>4</sub>]<sub>n</sub> network. Catalytic peroxidative oxidation activity of <strong>1</strong> and <strong>2</strong> was examined on the oxidation of benzyl alcohol using tertiary-butyl hydroperoxide (<em>t-</em>BuOOH) as the oxygen source. The compound <strong>1</strong> exhibited over 90 % product conversion at 80 °C in 24-hour reaction time. In addition, the catalyst exhibited high selectivity towards benzaldehyde and no over-oxidation product (benzoic acid) was detected.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117263"},"PeriodicalIF":2.4,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142552070","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 : 2024-10-22DOI: 10.1016/j.poly.2024.117262
Joseph O. Ogar, Toby J. Blundell, Rifna Usman, Marek Vavrovič, Lee Martin
Sodium salts of the spiroborate anion bis[(1,1′-binaphthalene)-2,2′-diolato-O,O’]borate in enantiopure and racemic forms have been obtained through reaction of BORAX (sodium tetraborate hexahydrate) with the corresponding stereoisomers of BINOL [(1,1′-binaphthalene)-2,2′-diol]. Electrocrystallisation of these salts with BEDT-TTF produces single crystals of a 1:1 radical-cation salt, (BEDT-TTF){B[1,1′-bis(BINOL)]2}•THF, with the racemic spiroborate anion whilst no crystals were obtained with the enantiopure forms.
{"title":"Chiral and racemic BINOL spiroborate anions and radical-cation salt with BEDT-TTF","authors":"Joseph O. Ogar, Toby J. Blundell, Rifna Usman, Marek Vavrovič, Lee Martin","doi":"10.1016/j.poly.2024.117262","DOIUrl":"10.1016/j.poly.2024.117262","url":null,"abstract":"<div><div>Sodium salts of the spiroborate anion bis[(1,1′-<em>binaphthalene</em>)-2,2′-<em>diolato</em>-<em>O</em>,<em>O</em>’]borate in enantiopure and racemic forms have been obtained through reaction of BORAX (sodium tetraborate hexahydrate) with the corresponding stereoisomers of BINOL [(1,1′-binaphthalene)-2,2′-diol]. Electrocrystallisation<!--> <!-->of these salts<!--> <!-->with BEDT-TTF produces single crystals of a 1:1 radical-cation salt, (BEDT-TTF){B[1,1′-bis(BINOL)]<sub>2</sub>}•THF, with the racemic spiroborate anion whilst no crystals were obtained with the enantiopure forms.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117262"},"PeriodicalIF":2.4,"publicationDate":"2024-10-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142531349","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Quantum chemical calculations were performed to study the binding affinity of the B3C2H5 cluster with noble gases. The results indicate that noble gas atoms especially the heavier ones such as Xe and Kr can form stable complexes with this cluster. Detailed analysis of the interaction mechanism reveals that the noble gas atoms serve as donor fragments in the formation of Ng@B3C2H5, 2Ng@B3C2H5, and 3Ng@B3C2H5 donor–acceptor complexes.
{"title":"Density functional theory investigation for noble gases adsorption on B3C2H5 structure","authors":"Esraa Kareem Sehen Bany Mshatat , Morteza Rouhani , Hamid Saeidian","doi":"10.1016/j.poly.2024.117266","DOIUrl":"10.1016/j.poly.2024.117266","url":null,"abstract":"<div><div>Quantum chemical calculations were performed to study the binding affinity of the B<sub>3</sub>C<sub>2</sub>H<sub>5</sub> cluster with noble gases. The results indicate that noble gas atoms especially the heavier ones such as Xe and Kr can form stable complexes with this cluster. Detailed analysis of the interaction mechanism reveals that the noble gas atoms serve as donor fragments in the formation of Ng@B<sub>3</sub>C<sub>2</sub>H<sub>5</sub>, 2Ng@B<sub>3</sub>C<sub>2</sub>H<sub>5</sub>, and 3Ng@B<sub>3</sub>C<sub>2</sub>H<sub>5</sub> donor–acceptor complexes.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117266"},"PeriodicalIF":2.4,"publicationDate":"2024-10-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142531447","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 : 2024-10-16DOI: 10.1016/j.poly.2024.117260
C.J. Ann Mary , Devipriya Vasudevan , Prasiddha Nagarajan , S. Suhas , Ajesh Vijayan , K.V. Radhakrishnan , Y.N. Sudhakar
The present review article explores the expansive synthetic methodologies facilitated by CH activation of indoles using transition metal catalysts. The strategic utilization of catalysts such as palladium, rhodium, iridium, ruthenium, and manganese has revolutionized organic synthesis by enabling selective alkynylation, acylation, and annulation reactions. These transformations are pivotal in pharmaceuticals, particularly in the synthesis of antihistamines and potential antiviral drugs against SARS-CoV-2. Additionally, these catalysts play a crucial role in perfumery and other chemical industries, enhancing the efficiency and precision of compound synthesis. The choice of transition metal catalysts is informed by their affordability and compatibility with both traditional analytical methods and innovative techniques like microwave synthesis and LED irradiation. Furthermore, this review underscores the interdisciplinary impact of transition metal-catalyzed CH activation on indoles, highlighting its significance in advancing both fundamental organic chemistry and applied sciences essential for modern technological advancements and drug discovery efforts.
本综述文章探讨了利用过渡金属催化剂对吲哚进行 CH 活化所促进的扩展合成方法。钯、铑、铱、钌和锰等催化剂的战略性使用，使选择性炔化、酰化和环化反应成为可能，从而彻底改变了有机合成。这些转化反应在制药领域，尤其是在合成抗组胺药和潜在的抗 SARS-CoV-2 病毒药物方面，具有举足轻重的作用。此外，这些催化剂在香水和其他化学工业中也发挥着至关重要的作用，可提高化合物合成的效率和精确度。选择过渡金属催化剂的依据是它们的经济性以及与传统分析方法和创新技术（如微波合成和 LED 照射）的兼容性。此外，本综述还强调了过渡金属催化 CH 活化对吲哚的跨学科影响，突出了其在推进基础有机化学和应用科学方面的重要意义，而基础有机化学和应用科学对于现代技术进步和药物发现工作至关重要。
{"title":"An extensive review on transition metal catalyzed indole CH activation: Catalyst selection and mechanistic insights","authors":"C.J. Ann Mary , Devipriya Vasudevan , Prasiddha Nagarajan , S. Suhas , Ajesh Vijayan , K.V. Radhakrishnan , Y.N. Sudhakar","doi":"10.1016/j.poly.2024.117260","DOIUrl":"10.1016/j.poly.2024.117260","url":null,"abstract":"<div><div>The present review article explores the expansive synthetic methodologies facilitated by C<img>H activation of indoles using transition metal catalysts. The strategic utilization of catalysts such as palladium, rhodium, iridium, ruthenium, and manganese has revolutionized organic synthesis by enabling selective alkynylation, acylation, and annulation reactions. These transformations are pivotal in pharmaceuticals, particularly in the synthesis of antihistamines and potential antiviral drugs against SARS-CoV-2. Additionally, these catalysts play a crucial role in perfumery and other chemical industries, enhancing the efficiency and precision of compound synthesis. The choice of transition metal catalysts is informed by their affordability and compatibility with both traditional analytical methods and innovative techniques like microwave synthesis and LED irradiation. Furthermore, this review underscores the interdisciplinary impact of transition metal-catalyzed C<img>H activation on indoles, highlighting its significance in advancing both fundamental organic chemistry and applied sciences essential for modern technological advancements and drug discovery efforts.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117260"},"PeriodicalIF":2.4,"publicationDate":"2024-10-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142531446","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-14DOI: 10.1016/j.poly.2024.117256
Simon Sengupta, Phil Liebing, Matthias Westerhausen
In the in situ Grignard Metalation Method (iGMM), intermediately formed ethylmagnesium bromide as well as ethylcalcium and ethylstrontium iodide metalate trialkylsilylethyne in THF. For Me3SiCCMgBr (1a) a temperature-dependent Schlenk equilibrium is operative and this heteroleptic compound coexists with the homoleptic congeners Mg(CCSiMe3)2 (1b) and MgBr2. The reaction enthalpy ΔH and entropy ΔS adopt characteristic values. Initially formed Me3SiCCCaI (2a) is quantitatively converted to the homoleptic compound Ca(CCSiMe3)2 (2b) and CaI2. With increasing size of the alkaline-earth metal increasing amounts of the degradation product Me3SiCCSiMe3 hamper isolation of analytically pure compounds of strontium and barium. The molecular structures of [(thf)3Mg(CCSiMe3)2] (1b) and [(thf)3Ca(µCCSiMe3)I]2 (2a) have been determined by single-crystal X-ray diffraction.
{"title":"In situ Grignard metalation method (iGMM) for the preparation of alkynyl magnesium and calcium compounds","authors":"Simon Sengupta, Phil Liebing, Matthias Westerhausen","doi":"10.1016/j.poly.2024.117256","DOIUrl":"10.1016/j.poly.2024.117256","url":null,"abstract":"<div><div>In the in situ Grignard Metalation Method (iGMM), intermediately formed ethylmagnesium bromide as well as ethylcalcium and ethylstrontium iodide metalate trialkylsilylethyne in THF. For Me<sub>3</sub>Si<img>C<img>C<img>MgBr (<strong>1a</strong>) a temperature-dependent Schlenk equilibrium is operative and this heteroleptic compound coexists with the homoleptic congeners Mg(C<img>C<img>SiMe<sub>3</sub>)<sub>2</sub> (<strong>1b</strong>) and MgBr<sub>2</sub>. The reaction enthalpy ΔH and entropy ΔS adopt characteristic values. Initially formed Me<sub>3</sub>Si<img>C<img>C<img>CaI (<strong>2a</strong>) is quantitatively converted to the homoleptic compound Ca(C<img>C<img>SiMe<sub>3</sub>)<sub>2</sub> (<strong>2b</strong>) and CaI<sub>2</sub>. With increasing size of the alkaline-earth metal increasing amounts of the degradation product Me<sub>3</sub>Si<img>C<img>C<img>SiMe<sub>3</sub> hamper isolation of analytically pure compounds of strontium and barium. The molecular structures of [(thf)<sub>3</sub>Mg(C<img>C<img>SiMe<sub>3</sub>)<sub>2</sub>] (<strong>1b</strong>) and [(thf)<sub>3</sub>Ca(µ<img>C<img>C<img>SiMe<sub>3</sub>)I]<sub>2</sub> (<strong>2a</strong>) have been determined by single-crystal X-ray diffraction.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117256"},"PeriodicalIF":2.4,"publicationDate":"2024-10-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142531445","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-12DOI: 10.1016/j.poly.2024.117255
Bibian Okokhere-Edeghoghon, Michael S. Hill, Mary F. Mahon
The reactivity of β-diketiminato alkylmagnesium, hydridomagnesium and hydridocalcium bases toward 1-methylimidazole, 1-tert-butylimidazole and 1-methylbenzimidazole enables the C-magnesiation and calciation of this family of N-heterocyclic molecules. Although 1-methylimidazole, 1-tert-butylimidazole, and 1-methylbenzimidazole are deprotonated at their C-2 positions by both the magnesium alkyl and hydride derivatives, these reagents can also leverage a level of regiodivergent kinetic discrimination and resultant C-4 metallation. In contrast to the straightforward C-2-deprotonation of 1-methylbenzimidazole provided by the magnesium hydride, a rapid cascade of apparent deprotonation, imidazole ring opening and twofold CC coupling was induced by the analogous calcium reagent. This process provides a tricalcium species comprising an unprecedented trianionic unit, which may be considered as a trimethylenemethane dianion isostere equipped with a pendent amide donor. While attempted boron functionalisation of the imidazolyl anions of the magnesium derivatives of 1-methylimidazole and 1-methylbenzimidazole with pinacolborane (HBpin) was unsuccessful, the 1-tert-butylimidazolyl analogue provided the C-2-borylated product irrespective of the position of initial C-2 or C-4 deprotonation. Although the calcium congeners resulting from 1-methylimidazole and 1-tert-butylimidazole were deduced to form similarly borylated products, study of their onward reactivity was prevented by their instability toward Schlenk-type redistribution in solution.
{"title":"Magnesiation and calciation of CH acidic N-alkyl imidazoles","authors":"Bibian Okokhere-Edeghoghon, Michael S. Hill, Mary F. Mahon","doi":"10.1016/j.poly.2024.117255","DOIUrl":"10.1016/j.poly.2024.117255","url":null,"abstract":"<div><div>The reactivity of β-diketiminato alkylmagnesium, hydridomagnesium and hydridocalcium bases toward 1-methylimidazole, 1-<em>tert</em>-butylimidazole and 1-methylbenzimidazole enables the <em>C-</em>magnesiation and calciation of this family of <em>N</em>-heterocyclic molecules. Although 1-methylimidazole, 1-<em>tert</em>-butylimidazole, and 1-methylbenzimidazole are deprotonated at their C-2 positions by both the magnesium alkyl and hydride derivatives, these reagents can also leverage a level of regiodivergent kinetic discrimination and resultant C-4 metallation. In contrast to the straightforward C-2-deprotonation of 1-methylbenzimidazole provided by the magnesium hydride, a rapid cascade of apparent deprotonation, imidazole ring opening and twofold C<img>C coupling was induced by the analogous calcium reagent. This process provides a tricalcium species comprising an unprecedented trianionic unit, which may be considered as a trimethylenemethane dianion isostere equipped with a pendent amide donor. While attempted boron functionalisation of the imidazolyl anions of the magnesium derivatives of 1-methylimidazole and 1-methylbenzimidazole with pinacolborane (HBpin) was unsuccessful, the 1-<em>tert-</em>butylimidazolyl analogue provided the C-2-borylated product irrespective of the position of initial C-2 or C-4 deprotonation. Although the calcium congeners resulting from 1-methylimidazole and 1-<em>tert-</em>butylimidazole were deduced to form similarly borylated products, study of their onward reactivity was prevented by their instability toward Schlenk-type redistribution in solution.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117255"},"PeriodicalIF":2.4,"publicationDate":"2024-10-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142445270","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A 2D open-framework zinc phosphate [C3N2H12][Zn2(HPO4)3] (1) was synthesized by solvothermal method. The inorganic anion layer is constructed from Zn2P2O12 cluster units and the interlayer spaces are filled by the diprotonated DAP molecules. The resultant compound had high purity and thermal stability by PXRD and TG analysis. This compound exhibited strongly temperature and humidity dependent proton conductivity, and its highest proton conductivity achieves 2.36 × 10−2 S.cm−1 at 100 %RH and 333 K. Moreover, the important effect of the dense hydrogen bond network in elevating the proton conductivity was explored through comparing the structure and proton conduction behavior between 1 and [C3N2H12][Zn(HPO4)2] (2), which synthesized via the same hydrothermal reaction process, and only a slight difference in the amount of DAP.
{"title":"A 2D open framework zinc phosphate and its high proton conductance properties at medium and low temperature","authors":"Kai-ming Zhang , Xiao-luo Zhong , Xue-yi Zhou , Xuan-ting Kuang , Hai-rong Zhao","doi":"10.1016/j.poly.2024.117258","DOIUrl":"10.1016/j.poly.2024.117258","url":null,"abstract":"<div><div>A 2D open-framework zinc phosphate <strong>[C<sub>3</sub>N<sub>2</sub>H<sub>12</sub>][Zn<sub>2</sub>(HPO<sub>4</sub>)<sub>3</sub>]</strong> (<strong>1</strong>) was synthesized by solvothermal method. The inorganic anion layer is constructed from Zn<sub>2</sub>P<sub>2</sub>O<sub>12</sub> cluster units and the interlayer spaces are filled by the diprotonated DAP molecules. The resultant compound had high purity and thermal stability by PXRD and TG analysis. This compound exhibited strongly temperature and humidity dependent proton conductivity, and its highest proton conductivity achieves 2.36 × 10<sup>−2</sup> S<sup>.</sup>cm<sup>−1</sup> at 100 %RH and 333 K. Moreover, the important effect of the dense hydrogen bond network in elevating the proton conductivity was explored through comparing the structure and proton conduction behavior between <strong>1</strong> and <strong>[C<sub>3</sub>N<sub>2</sub>H<sub>12</sub>][Zn(HPO<sub>4</sub>)<sub>2</sub>]</strong> (<strong>2</strong>), which synthesized <em>via</em> the same hydrothermal reaction process, and only a slight difference in the amount of DAP.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"264 ","pages":"Article 117258"},"PeriodicalIF":2.4,"publicationDate":"2024-10-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142552069","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, novel cyclotriphosphazene derivatives, {[N3P3(biph)(BA)2] (6a/b), [N3P3(biph)(BA)3] (7), [N3P3(biph)2(BA)Cl (8) and [N3P3(biph)2(BA)2 (9)]}, (biph = 2′,2′′-dioxy-1′,1′′- biphenyl, BA = butylated oxyanisole}, were synthesized from the nucleophilic substitution reactions of butylated hydroxyanisole (BHA) (5) with [N3P3(biph)Cl4] (3) and [N3P3(biph)2Cl2] (4), respectively. The structures of all the products (6a/b, 7, 8 and 9) were determined -using elemental analysis, mass and (1H and 31P) NMR spectroscopic techniques. The molecular and crystal structure of compound 9 was also determined by single crystal X-ray crystallography. At the same time, the compounds (3, 4, 7, 8 and 9) were tested for their antimicrobial and antioxidant (free radical scavenging) activities. Of all, compounds 8 and 9 showed relatively significant antimicrobial activity against the control strains Bacillus cereus DSMZ 4312 (16,5 and 18,25 mm) and against Staphylococcus aureus ATCC 29213 (25 and 22,5 mm) compared to their positive controls. The MIC50 values of compounds 8 and 9 against Bacillus cereus were determined at 125 µg/mL and < 325 µg/mL, respectively, and Staphylococcus aureus at 125 µg/ mL for both compounds. While the other compounds (3, 4 and 7) did not possess antimicrobial properties, they showed strong antioxidant activity. In the antioxidant assay based on the EC50 value of BHA used as a control, compound 7 showed antioxidant activity even at low concentrations such as 9,37 µg/ mL (83 %), while compounds 3 and 4 showed antioxidant properties even at relatively low concentrations such as 18,75 µg/mL. Compounds 8 and 9, two antimicrobial compounds, did not exhibit antioxidant properties.
{"title":"Synthesis and characterization of novel spiro-(2,2′-dioxybiphenyl)-cyclotriphosphazene derivatives bearing butylated oxyanisole groups and their antioxidant and antimicrobial activities","authors":"Efe Bilal Sönmez , Şule Şahin Ün , Ceylan Mutlu Balcı , Devrim Atilla , Mine Gül Şeker , Hanife İbişoğlu","doi":"10.1016/j.poly.2024.117252","DOIUrl":"10.1016/j.poly.2024.117252","url":null,"abstract":"<div><div>In this study, novel cyclotriphosphazene derivatives, {[N<sub>3</sub>P<sub>3</sub>(biph)(BA)<sub>2</sub>] (<strong>6a/b</strong>), [N<sub>3</sub>P<sub>3</sub>(biph)(BA)<sub>3</sub>] (<strong>7</strong>), [N<sub>3</sub>P<sub>3</sub>(biph)<sub>2</sub>(BA)Cl (<strong>8</strong>) and [N<sub>3</sub>P<sub>3</sub>(biph)<sub>2</sub>(BA)<sub>2</sub> (<strong>9</strong>)]}, (biph = 2′,2′′-dioxy-1′,1′′- biphenyl, BA = butylated oxyanisole}, were synthesized from the nucleophilic substitution reactions of butylated hydroxyanisole (BHA) (<strong>5</strong>) with [N<sub>3</sub>P<sub>3</sub>(biph)Cl<sub>4</sub>] (<strong>3</strong>) and [N<sub>3</sub>P<sub>3</sub>(biph)<sub>2</sub>Cl<sub>2</sub>] (<strong>4</strong>), respectively. The structures of all the products (<strong>6a/b</strong>, <strong>7</strong>, <strong>8</strong> and <strong>9</strong>) were determined -using elemental analysis, mass and (<sup>1</sup>H and <sup>31</sup>P) NMR spectroscopic techniques. The molecular and crystal structure of compound <strong>9</strong> was also determined by single crystal X-ray crystallography. At the same time, the compounds (<strong>3</strong>, <strong>4</strong>, <strong>7</strong>, <strong>8</strong> and <strong>9</strong>) were tested for their antimicrobial and antioxidant (free radical scavenging) activities. Of all, compounds <strong>8</strong> and <strong>9</strong> showed relatively significant antimicrobial activity against the control strains <em>Bacillus cereus</em> DSMZ 4312 (16,5 and 18,25 mm) and against <em>Staphylococcus aureus</em> ATCC 29213 (25 and 22,5 mm) compared to their positive controls. The MIC<sub>50</sub> values of compounds <strong>8</strong> and <strong>9</strong> against <em>Bacillus cereus</em> were determined at 125 µg/mL and < 325 µg/mL, respectively, and <em>Staphylococcus aureus</em> at 125 µg/ mL for both compounds. While the other compounds (<strong>3</strong>, <strong>4</strong> and <strong>7</strong>) did not possess antimicrobial properties, they showed strong antioxidant activity. In the antioxidant assay based on the EC<sub>50</sub> value of BHA used as a control, compound <strong>7</strong> showed antioxidant activity even at low concentrations such as 9,37 µg/ mL (83 %), while compounds <strong>3</strong> and <strong>4</strong> showed antioxidant properties even at relatively low concentrations such as 18,75 µg/mL. Compounds <strong>8</strong> and <strong>9</strong>, two antimicrobial compounds, did not exhibit antioxidant properties.</div></div>","PeriodicalId":20278,"journal":{"name":"Polyhedron","volume":"265 ","pages":"Article 117252"},"PeriodicalIF":2.4,"publicationDate":"2024-10-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142653682","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 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}
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