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Revealing a new electroneutral uranium oxide hydrate phase with a framework structure in triclinic space group
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-22 DOI: 10.1016/j.ica.2025.122611
Yingjie Zhang, Timothy A. Ablott, Tao Wei
Uranium hydrolysis processes and associated products are fundamentally important especially to uranium geochemistry and the nuclear fuel cycle. Herein, we report the formation and characterisation of a new electroneutral uranium oxide hydrate framework (UOHF), U(H2O)8[(UO2)10UO13(OH)4] (UOHF2), using both structural and spectroscopic techniques. As a minor phase from the hydrothermal uranium hydrolysis in the presence of Cu(II) ions, compound UOHF2 crystallises in the triclinic P1¯ space group having a framework structure constructed with β-U3O8 type layers pillared by double pentagonal uranium bipyramids and tetravalent U(IV) ions sitting inside the framework channels. The crystal structure has been revealed using synchrotron single crystal X-ray diffraction and confirmed by electron diffraction with transmission electron microscopy. The characteristic vibrational modes due to the presence of various hexavalent uranium centres were revealed by Raman spectroscopy. The successful synthesis and characterisation of UOHF2, together with an earlier reported U(H2O)2[(UO2)10O10(OH)2(UO4)(H2O)2] (UOHF1), highlights the complex nature of uranium hydrolysis processes and its related products, with direct implications to fundamental uranium chemistry, geochemistry and the current nuclear fuel cycle.
{"title":"Revealing a new electroneutral uranium oxide hydrate phase with a framework structure in triclinic space group","authors":"Yingjie Zhang,&nbsp;Timothy A. Ablott,&nbsp;Tao Wei","doi":"10.1016/j.ica.2025.122611","DOIUrl":"10.1016/j.ica.2025.122611","url":null,"abstract":"<div><div>Uranium hydrolysis processes and associated products are fundamentally important especially to uranium geochemistry and the nuclear fuel cycle. Herein, we report the formation and characterisation of a new electroneutral uranium oxide hydrate framework (UOHF), U(H<sub>2</sub>O)<sub>8</sub>[(UO<sub>2</sub>)<sub>10</sub>UO<sub>13</sub>(OH)<sub>4</sub>] (<strong>UOHF2</strong>), using both structural and spectroscopic techniques. As a minor phase from the hydrothermal uranium hydrolysis in the presence of Cu(II) ions, compound <strong>UOHF2</strong> crystallises in the triclinic <em>P</em><span><math><mover><mn>1</mn><mo>¯</mo></mover></math></span> space group having a framework structure constructed with β-U<sub>3</sub>O<sub>8</sub> type layers pillared by double pentagonal uranium bipyramids and tetravalent U(IV) ions sitting inside the framework channels. The crystal structure has been revealed using synchrotron single crystal X-ray diffraction and confirmed by electron diffraction with transmission electron microscopy. The characteristic vibrational modes due to the presence of various hexavalent uranium centres were revealed by Raman spectroscopy. The successful synthesis and characterisation of <strong>UOHF2</strong>, together with an earlier reported U(H<sub>2</sub>O)<sub>2</sub>[(UO<sub>2</sub>)<sub>10</sub>O<sub>10</sub>(OH)<sub>2</sub>(UO<sub>4</sub>)(H<sub>2</sub>O)<sub>2</sub>] (<strong>UOHF1</strong>), highlights the complex nature of uranium hydrolysis processes and its related products, with direct implications to fundamental uranium chemistry, geochemistry and the current nuclear fuel cycle.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122611"},"PeriodicalIF":2.7,"publicationDate":"2025-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143521040","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}
引用次数: 0
One-pot synthesis of 2,4,5-triarylimidazole and phenanthro[9,10-d]imidazole derivatives catalyzed by a new set of crystalline aluminium(III) complexes via CN bond formation
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-21 DOI: 10.1016/j.ica.2025.122596
Mahabarathi Subramaniyan, Madhvesh Pathak
A series of three new along with one existing hexacoordinated heteroleptic derivatives of aluminium(III) as [(C6H5COCHCOC6H5)Al(1a-1d)].H2O {where 1a-1d are dianionic [ONO]-tridentate ancillary ligands} was synthesized quantitively by treating Al(OPri)3 with Schiff bases (1a-1d) and dibenzoyl methane in a 1:1:1 ratio using anhydrous benzene as a solvent. As 2a was already reported by this research team only so the new derivatives (2b-2d) were characterized using appropriate analytical techniques such as FTIR, UV–Vis, NMR (1H, 13C & DEPT-135) and HRMS. Specifically, SC-XRD authenticated the molecular structures of complexes of 2a, 2b and 2d. The developed crystals verified the hexacoordination around the central metal aluminium encircled with five oxygen atoms and one that of nitrogen. These trio crystals appeared as triclinic with a space group of P1¯ and Z values 2, 4 and 4, respectively. Subsequently, computational investigation of the aluminium(III) derivatives was carried out using DFT/B3LYP/LanL2DZ method in Gaussian(09) software. Further, the optimized molecular structures were derived from B3LYP/6-311G(d,p) and the results were rationalized with the support of TD-DFT calculations. Afterwards, synthesis of a substituted five membered heterocyclic compounds were carried out in an ethanolic solution of benzil/9,10-phenanthrenequinone, substituted aldehydes and ammonium acetate (nitrogen source) as a substrate while employing aforementioned all four aluminium(III) complexes as catalyst. These organic compounds were characterized by spectral tools like NMR (1H & 13C) and FTIR. Furthermore, nitro derivative 6c’ was validated by SC-XRD that appeared as monoclinic system with space group of P21/n. This study is the foremost approach to utilize aluminium(III) complexes as catalyst for the condensation reaction of 2,4,5-triarylimidazole and phenanthro[9,10-d]imidazole where obtained organic derivatives were synthesized in 83–95 % yields.
{"title":"One-pot synthesis of 2,4,5-triarylimidazole and phenanthro[9,10-d]imidazole derivatives catalyzed by a new set of crystalline aluminium(III) complexes via CN bond formation","authors":"Mahabarathi Subramaniyan,&nbsp;Madhvesh Pathak","doi":"10.1016/j.ica.2025.122596","DOIUrl":"10.1016/j.ica.2025.122596","url":null,"abstract":"<div><div>A series of three new along with one existing hexacoordinated heteroleptic derivatives of aluminium(III) as <strong>[(C</strong><sub><strong>6</strong></sub><strong>H</strong><sub><strong>5</strong></sub><strong>COCHCOC</strong><sub><strong>6</strong></sub><strong>H</strong><sub><strong>5</strong></sub><strong>)Al(1a-1d)].H</strong><sub><strong>2</strong></sub><strong>O {</strong>where <strong>1a-1d</strong> are dianionic [ONO]-tridentate ancillary ligands} was synthesized quantitively by treating Al(OPr<sup><em>i</em></sup>)<sub>3</sub> with Schiff bases (<strong>1a-1d</strong>) and dibenzoyl methane in a 1:1:1 ratio using anhydrous benzene as a solvent. As <strong>2a</strong> was already reported by this research team only so the new derivatives (<strong>2b-2d</strong>) were characterized using appropriate analytical techniques such as FTIR, UV–Vis, NMR (<sup>1</sup>H, <sup>13</sup>C &amp; DEPT-135) and HRMS. Specifically, SC-XRD authenticated the molecular structures of complexes of <strong>2a, 2b</strong> and <strong>2d</strong>. The developed crystals verified the hexacoordination around the central metal aluminium encircled with five oxygen atoms and one that of nitrogen. These trio crystals appeared as triclinic with a space group of <em>P</em><span><math><mover><mrow><mn>1</mn><mspace></mspace></mrow><mo>¯</mo></mover></math></span> and Z values 2, 4 and 4, respectively<em>.</em> Subsequently, computational investigation of the aluminium(III) derivatives was carried out using DFT/B3LYP/LanL2DZ method in Gaussian(09) software. Further, the optimized molecular structures were derived from B3LYP/6-311G(d,p) and the results were rationalized with the support of TD-DFT calculations. Afterwards, synthesis of a substituted five membered heterocyclic compounds were carried out in an ethanolic solution of benzil/9,10-phenanthrenequinone, substituted aldehydes and ammonium acetate (nitrogen source) as a substrate while employing aforementioned all four aluminium(III) complexes as catalyst. These organic compounds were characterized by spectral tools like NMR (<sup>1</sup>H &amp; <sup>13</sup>C) and FTIR. Furthermore, nitro derivative <strong>6c’</strong> was validated by SC-XRD that appeared as monoclinic system with space group of <em>P</em>2<sub>1</sub>/n. This study is the foremost approach to utilize aluminium(III) complexes as catalyst for the condensation reaction of 2,4,5-triarylimidazole and phenanthro[9,10-<em>d</em>]imidazole where obtained organic derivatives were synthesized in 83–95 % yields.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122596"},"PeriodicalIF":2.7,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143510949","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}
引用次数: 0
Preparation of lanthanum and nickel complexes based on a newly prepared Schiff base ligand: Structural elucidation, molecular docking, and density functional theory calculations
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-21 DOI: 10.1016/j.ica.2025.122602
Sabrein H. Mohamed , Tarek A. Yousef , Ramy A. Bedier , Ibtisam Alali , Tamer H.A. Hasanin , Rania H. Taha
This study describes the synthesis of new Lanthanum (La) and Nickel (Ni) complexes using a novel Schiff base ligand derived from the condensation reaction of 4-aminoantipyrine, 5-bromosalicylaldehyde, and o-phenylenediamine. The Schiff base ligand was characterized using various spectroscopic techniques, such as 1H and 13C NMR spectroscopy, and UV–visible spectral studies, to confirm its structure and purity. The metal complexes were prepared by reacting the ligand with LaNO3.6H2O and NiCl2.6H2O under reflux conditions, and their structural properties were determined through 1H and 13C NMR spectroscopy. Density Functional Theory (DFT) calculations were employed to investigate the geometry and electronic structure of the complexes, providing insights into their stability, frontier molecular orbitals (HOMO-LUMO), and reactivity indices. DFT analysis showed that the La complex forms the strongest bond with the ligand, indicated by its higher binding energy compared to the Ni complex. HOMO and LUMO energy gap levels indicate that the Ni complex is the most reactive compound, while the La complex exhibits lower reactivity due to its larger energy gap. Molecular docking studies were conducted to assess the biological activity of the Schiff base ligand and its complexes against the active sites of Entamoeba coli (ID: 1C14) as Gram-negative bacteria, Staphylococcus aureus (ID: 2XCT) as Gram-positive bacteria, and Xanthine oxidase (ID: 1FIQ) as an antioxidant agent protein-selected biological target, revealing strong binding interactions that suggest potential applications as antimicrobial or anticancer agents. Overall, this study demonstrates the successful synthesis and characterization of Lanthanum and Nickel complexes, supported by computational analyses, and highlights their promising biological relevance, opening up avenues for further research in medicinal chemistry and materials science.
本研究介绍了利用一种新型希夫碱配体合成新的镧(La)和镍(Ni)配合物的过程,这种新型希夫碱配体来自 4-氨基安替比林、5-溴水杨醛和邻苯二胺的缩合反应。为了确认希夫碱配体的结构和纯度,使用了各种光谱技术(如 1H 和 13C NMR 光谱以及紫外-可见光谱研究)对其进行了表征。配体与 LaNO3.6H2O 和 NiCl2.6H2O 在回流条件下反应制备了金属配合物,并通过 1H 和 13C NMR 光谱测定了它们的结构特性。利用密度泛函理论(DFT)计算研究了这些配合物的几何和电子结构,深入了解了它们的稳定性、前沿分子轨道(HOMO-LUMO)和反应性指数。DFT 分析表明,与 Ni 复合物相比,La 复合物的结合能更高,表明它与配体形成的键最强。HOMO 和 LUMO 能隙水平表明,Ni 复合物是反应性最强的化合物,而 La 复合物由于能隙较大而表现出较低的反应性。分子对接研究评估了希夫碱配体及其配合物对革兰氏阴性菌大肠杆菌(ID:1C14)、革兰氏阳性菌金黄色葡萄球菌(ID:2XCT)以及抗氧化剂蛋白质选定生物靶点黄嘌呤氧化酶(ID:1FIQ)活性位点的生物活性,结果显示,这些配体与靶点之间存在很强的结合相互作用,具有作为抗菌剂或抗癌剂的潜在应用前景。总之,本研究在计算分析的支持下,成功地合成了镧镍配合物,并对其进行了表征,同时强调了它们具有良好的生物学相关性,为进一步开展药物化学和材料科学研究开辟了道路。
{"title":"Preparation of lanthanum and nickel complexes based on a newly prepared Schiff base ligand: Structural elucidation, molecular docking, and density functional theory calculations","authors":"Sabrein H. Mohamed ,&nbsp;Tarek A. Yousef ,&nbsp;Ramy A. Bedier ,&nbsp;Ibtisam Alali ,&nbsp;Tamer H.A. Hasanin ,&nbsp;Rania H. Taha","doi":"10.1016/j.ica.2025.122602","DOIUrl":"10.1016/j.ica.2025.122602","url":null,"abstract":"<div><div>This study describes the synthesis of new Lanthanum (La) and Nickel (Ni) complexes using a novel Schiff base ligand derived from the condensation reaction of 4-aminoantipyrine, 5-bromosalicylaldehyde, and <em>o</em>-phenylenediamine. The Schiff base ligand was characterized using various spectroscopic techniques, such as <sup>1</sup>H and <sup>13</sup>C NMR spectroscopy, and UV–visible spectral studies, to confirm its structure and purity. The metal complexes were prepared by reacting the ligand with LaNO<sub>3</sub>.6H<sub>2</sub>O and NiCl<sub>2</sub>.6H<sub>2</sub>O under reflux conditions, and their structural properties were determined through <sup>1</sup>H and <sup>13</sup>C NMR spectroscopy. Density Functional Theory (DFT) calculations were employed to investigate the geometry and electronic structure of the complexes, providing insights into their stability, frontier molecular orbitals (HOMO-LUMO), and reactivity indices. DFT analysis showed that the La complex forms the strongest bond with the ligand, indicated by its higher binding energy compared to the Ni complex. HOMO and LUMO energy gap levels indicate that the Ni complex is the most reactive compound, while the La complex exhibits lower reactivity due to its larger energy gap. Molecular docking studies were conducted to assess the biological activity of the Schiff base ligand and its complexes against the active sites of <em>Entamoeba coli</em> (ID: 1C14) as Gram-negative bacteria, <em>Staphylococcus aureus</em> (ID: 2XCT) as Gram-positive bacteria, and Xanthine oxidase (ID: 1FIQ) as an antioxidant agent protein-selected biological target, revealing strong binding interactions that suggest potential applications as antimicrobial or anticancer agents. Overall, this study demonstrates the successful synthesis and characterization of Lanthanum and Nickel complexes, supported by computational analyses, and highlights their promising biological relevance, opening up avenues for further research in medicinal chemistry and materials science.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122602"},"PeriodicalIF":2.7,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143480091","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}
引用次数: 0
Fabrication of cu(II)-coordination polymer and its Mn-doped composites for luminescent detection of Novaluron pesticide, La3+ and TEA
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-19 DOI: 10.1016/j.ica.2025.122599
Anat Ram Sidar , Musheer Ahmad , Nazrul Haq , Astakala Anil Kumar , Kafeel Ahmad Siddiqui
A new copper-based coordination polymer, [Cu₃(Timb)₂(OA)₂·6(H₂O)]ₙ (1), was synthesized using 1,3,5-tris[(1H-imidazol-1-yl)methyl]benzene (Timb) and orotic acid (OA) ligands. The structure of (1) was characterized through single-crystal X-ray diffraction (SCXRD), Thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDX), and powder X-ray diffraction (PXRD). To enhance its luminescent properties, the polymer was doped with MnO2, MnO@Cu-CP-2 (2), which was further characterized by FTIR, PXRD, TGA, and SEM-EDX. Both the undoped (1) and doped (2) materials exhibited promising luminescent properties for detecting triethylamine (TEA), La3+ ions, MnO4, and hazardous pesticides such as Novaluron (NVR). Detection limits for (1) were determined to be 0.1405 ppm, 0.2321 ppm, 0.6601 ppm, and 0.7242 ppm for TEA, La3+, MnO4, and NVR, respectively. Upon MnO2 doping, (2) demonstrated enhanced luminescent sensing capabilities, with detection limits of 0.4067 ppm, 0.6625 ppm, 0.9363 ppm, and 0.9862 ppm for the same analytes. The study also provides detailed insights into the luminescence mechanisms and the role of MnO2 incorporation in enhancing the sensing performance, underscoring the potential of (2) for superior analytes detection compared to the undoped polymer.
{"title":"Fabrication of cu(II)-coordination polymer and its Mn-doped composites for luminescent detection of Novaluron pesticide, La3+ and TEA","authors":"Anat Ram Sidar ,&nbsp;Musheer Ahmad ,&nbsp;Nazrul Haq ,&nbsp;Astakala Anil Kumar ,&nbsp;Kafeel Ahmad Siddiqui","doi":"10.1016/j.ica.2025.122599","DOIUrl":"10.1016/j.ica.2025.122599","url":null,"abstract":"<div><div>A new copper-based coordination polymer, <strong>[Cu₃(Timb)₂(OA)₂·6(H₂O)]ₙ</strong> (<strong>1</strong>), was synthesized using 1,3,5-tris[(1H-imidazol-1-yl)methyl]benzene (Timb) and orotic acid (OA) ligands. The structure of (<strong>1</strong>) was characterized through single-crystal X-ray diffraction (SCXRD), Thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDX), and powder X-ray diffraction (PXRD). To enhance its luminescent properties, the polymer was doped with MnO<sub>2</sub>, <strong>MnO@Cu-CP-2 (2)</strong>, which was further characterized by FTIR, PXRD, TGA, and SEM-EDX. Both the undoped (<strong>1</strong>) and doped (<strong>2</strong>) materials exhibited promising luminescent properties for detecting triethylamine (TEA), La<sup>3+</sup> ions, MnO<sub>4</sub><sup>−</sup>, and hazardous pesticides such as Novaluron (NVR). Detection limits for (<strong>1</strong>) were determined to be 0.1405 ppm, 0.2321 ppm, 0.6601 ppm, and 0.7242 ppm for TEA, La<sup>3+</sup>, MnO<sub>4</sub><sup>−</sup>, and NVR, respectively. Upon MnO<sub>2</sub> doping, (<strong>2</strong>) demonstrated enhanced luminescent sensing capabilities, with detection limits of 0.4067 ppm, 0.6625 ppm, 0.9363 ppm, and 0.9862 ppm for the same analytes. The study also provides detailed insights into the luminescence mechanisms and the role of MnO<sub>2</sub> incorporation in enhancing the sensing performance, underscoring the potential of <strong>(2)</strong> for superior analytes detection compared to the undoped polymer.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122599"},"PeriodicalIF":2.7,"publicationDate":"2025-02-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143465401","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}
引用次数: 0
Synthesis of a dinuclear bis(μ-tetrazolato)dicobalt(III) Schiff base complex via tandem 1,3-dipolar cycloaddition: Formation of a supramolecular 1D polymer by the combination of the H-bonds, π-stacking, and π-hole interactions
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-18 DOI: 10.1016/j.ica.2025.122595
Susovan Bera , Antonio Frontera , Shouvik Chattopadhyay
A dinuclear and bis(μ-tetrazolato) bridged cobat (III) Schiff base complex, [(μ-N3)(μ-MTZ){CoN3(L)}2] {where HL = ((2-(dimethylamino)ethylimino)methyl)-4-bromophenol, and HMTZ = 5-methyl tetrazolate}, has been synthesized by in situ 1,3-dipolar cycloaddition and characterized by elemental and spectral analysis, and by X-ray crystallography. The complex crystallizes in orthorhombic space group Pna21. The complex features a double μ-NN’-tetrazolato bridged dicobalt(III) structure, in which each cobalt(III) is octahedral being coordinated by a depronated NNO-donor terdentate Schiff base (L) in meridional fashion, one terminal azide, one end-on bridging azide and one nitrogen atom of the bridging (MTZ). The ability of the three azide ligands to participate in H-bonding interactions as acceptor is analyzed using DFT calculations and several computational tools including MEP, QTAIM and NCIplot.
通过原位 1,3-二极环加成法合成了一种双核双(μ-四唑)桥接钴酸酯(III)希夫碱配合物 [(μ-N3)(μ-MTZ){CoN3(L)}2] { 其中 HL = ((2-(dimethylamino)ethylimino)methyl)-4-bromophenol、和 HMTZ = 5-甲基四唑醇},通过原位 1,3-二极环加成法合成,并通过元素分析、光谱分析和 X 射线晶体学进行了表征。该复合物在正交空间群 Pna21 中结晶。该复合物具有双μ-NN'-四氮唑桥联的二钴(III)结构,其中每个钴(III)都是八面体,由一个去质子化的 NNO 供体三齿席夫碱 (L-)、一个末端叠氮化物、一个末端桥联叠氮化物和一个桥联 (MTZ)- 的氮原子以经向方式配位。利用 DFT 计算和多种计算工具(包括 MEP、QTAIM 和 NCIplot)分析了这三种叠氮配体作为受体参与 H 键相互作用的能力。
{"title":"Synthesis of a dinuclear bis(μ-tetrazolato)dicobalt(III) Schiff base complex via tandem 1,3-dipolar cycloaddition: Formation of a supramolecular 1D polymer by the combination of the H-bonds, π-stacking, and π-hole interactions","authors":"Susovan Bera ,&nbsp;Antonio Frontera ,&nbsp;Shouvik Chattopadhyay","doi":"10.1016/j.ica.2025.122595","DOIUrl":"10.1016/j.ica.2025.122595","url":null,"abstract":"<div><div>A dinuclear and bis(μ-tetrazolato) bridged cobat (III) Schiff base complex, <strong><em>[(μ-N</em></strong><sub><strong><em>3</em></strong></sub><strong><em>)</em></strong>(μ-MTZ){<strong><em>CoN</em></strong><sub><strong><em>3</em></strong></sub><strong><em>(L)}</em></strong><sub><strong><em>2</em></strong></sub><strong><em>]</em></strong> {where HL = <em>((2-(dimethylamino)ethylimino)methyl)-4-bromophenol</em>, and HMTZ = 5-methyl tetrazolate}, has been synthesized by in situ 1,3-dipolar cycloaddition and characterized by elemental and spectral analysis, and by X-ray crystallography. The complex crystallizes in orthorhombic space group <em>Pna2</em><sub><em>1</em></sub>. The complex features a double μ-NN’-tetrazolato bridged dicobalt(III) structure, in which each cobalt(III) is octahedral being coordinated by a depronated NNO-donor terdentate Schiff base (L<sup>−</sup>) in meridional fashion, one terminal azide, one end-on bridging azide and one nitrogen atom of the bridging (MTZ)<sup>−</sup>. The ability of the three azide ligands to participate in H-bonding interactions as acceptor is analyzed using DFT calculations and several computational tools including MEP, QTAIM and NCIplot.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122595"},"PeriodicalIF":2.7,"publicationDate":"2025-02-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143480089","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}
引用次数: 0
Recent strategies and developments in the hydroboration of N-Heteroarenes mediated by transition and rare-earth metal complexes 过渡金属和稀土金属络合物介导的 N-异戊二烯氢硼化合反应的最新策略和进展
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-15 DOI: 10.1016/j.ica.2025.122594
Priyanka Velmurugan , Moris S. Eisen , Tapas Ghatak
The dearomatization reactions of N-heteroarenes have emerged as crucial chemical transformations in the fields of organic synthesis and medicinal chemistry. These reactions permit the formation of aza compounds, including dihydropyridines, which serve as versatile synthetic building blocks and structural motifs for various bioactive natural products and pharmaceuticals. Over the past few years, dearomative hydroboration has grown into a powerful alternative to traditional reduction methods for N-heteroarenes. This option has demonstrated exceptional selectivity and a high tolerance for different functional groups, indicating great promise. This review provides an emerging overview of selective dearomative hydroboration reactions of N-heterocycles, including pyridines and quinolines. This review encompasses the period from 2014 to the present, examining 31 highly effective catalytic systems that feature d- and f-block metal complexes.
{"title":"Recent strategies and developments in the hydroboration of N-Heteroarenes mediated by transition and rare-earth metal complexes","authors":"Priyanka Velmurugan ,&nbsp;Moris S. Eisen ,&nbsp;Tapas Ghatak","doi":"10.1016/j.ica.2025.122594","DOIUrl":"10.1016/j.ica.2025.122594","url":null,"abstract":"<div><div>The dearomatization reactions of N-heteroarenes have emerged as crucial chemical transformations in the fields of organic synthesis and medicinal chemistry. These reactions permit the formation of aza compounds, including dihydropyridines, which serve as versatile synthetic building blocks and structural motifs for various bioactive natural products and pharmaceuticals. Over the past few years, dearomative hydroboration has grown into a powerful alternative to traditional reduction methods for N-heteroarenes. This option has demonstrated exceptional selectivity and a high tolerance for different functional groups, indicating great promise. This review provides an emerging overview of selective dearomative hydroboration reactions of N-heterocycles, including pyridines and quinolines. This review encompasses the period from 2014 to the present, examining 31 highly effective catalytic systems that feature d- and f-block metal complexes.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122594"},"PeriodicalIF":2.7,"publicationDate":"2025-02-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143446068","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}
引用次数: 0
A highly cytotoxic Pd(II) saccharinate complex with tris(2-pyridylmethyl)amine acting through mitochondrial and ROS-induced DNA damage
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-13 DOI: 10.1016/j.ica.2025.122590
Ceyda Icsel , Seyma Aydinlik , Muhittin Aygun , Veysel T. Yilmaz
A novel Pd(II) complex containing saccharinate (sac) and tris(2-pyridylmethyl)amine (tpma) [Pd (sac)(tpma)](sac)⋅1.5H2O was synthesized and characterized by IR, ESI-MS, NMR spectroscopic methods, DTA/TG thermal analysis methods and single-crystal X-ray diffraction.
The cationic Pd(II) complex displayed a distorted square planar coordination geometry with a N atom of sac and three N atoms of tpma, while another sac remained outside the coordination sphere as a counter ion. The sulforhodamine B (SRB) cell viability assay showed that the Pd(II) complex was found to be highly cytotoxic against four human cancer cell lines A549 (lung), HT29 (colon), MCF7 (breast), and LNCaP (prostate) in comparison with cisplatin. The complex demonstrated a remarkable selectivity toward MCF7 cells. Mechanistic studies indicated that the complex induced apoptosis in MCF7 cells based on annexin V/PI and caspase 3/7 assays. In addition, significant mitochondrial depolarization and increased intracellular ROS (reactive oxygen species) generation were observed in MCF7 cells exposed to the Pd(II) complex. The complex also caused ROS-induced DNA double strand breaks as evidenced by the γ-H2AX assay.
{"title":"A highly cytotoxic Pd(II) saccharinate complex with tris(2-pyridylmethyl)amine acting through mitochondrial and ROS-induced DNA damage","authors":"Ceyda Icsel ,&nbsp;Seyma Aydinlik ,&nbsp;Muhittin Aygun ,&nbsp;Veysel T. Yilmaz","doi":"10.1016/j.ica.2025.122590","DOIUrl":"10.1016/j.ica.2025.122590","url":null,"abstract":"<div><div>A novel Pd(II) complex containing saccharinate (sac) and tris(2-pyridylmethyl)amine (tpma) [Pd (sac)(tpma)](sac)⋅1.5H<sub>2</sub>O was synthesized and characterized by IR, ESI-MS, NMR spectroscopic methods, DTA/TG thermal analysis methods and single-crystal X-ray diffraction.</div><div>The cationic Pd(II) complex displayed a distorted square planar coordination geometry with a N atom of sac and three N atoms of tpma, while another sac remained outside the coordination sphere as a counter ion. The sulforhodamine B (SRB) cell viability assay showed that the Pd(II) complex was found to be highly cytotoxic against four human cancer cell lines A549 (lung), HT29 (colon), MCF7 (breast), and LNCaP (prostate) in comparison with cisplatin. The complex demonstrated a remarkable selectivity toward MCF7 cells. Mechanistic studies indicated that the complex induced apoptosis in MCF7 cells based on annexin V/PI and caspase 3/7 assays. In addition, significant mitochondrial depolarization and increased intracellular ROS (reactive oxygen species) generation were observed in MCF7 cells exposed to the Pd(II) complex. The complex also caused ROS-induced DNA double strand breaks as evidenced by the γ-H2AX assay.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122590"},"PeriodicalIF":2.7,"publicationDate":"2025-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143429354","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}
引用次数: 0
Synthesis and biological assay of biopolymeric chitosan functionalized by phosphoramidic segment P(O)[NH-3Py]2 and its Cu(II), Ni(II) and Hg(II) complexes
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-13 DOI: 10.1016/j.ica.2025.122593
Zeinab Albobaledi , Atekeh Tarahhomi , Ali Khaleghian , Negar Sarmadi
Biopolymeric chitosan-phosphoramide (CPA) and its complexes of Cu(II), Ni(II) and Hg(II) were synthesized and characterized by techniques of FT-IR, elemental analysis (CHN), thermogravimetric analysis (TGA), powder X-ray diffraction (PXRD) and scanning electron microscope (SEM). The cytotoxicity of these compounds against breast MDA-MB-231 cell lines was assessed by MTT assay, where the CPA-Hg(II) complex with an IC50 of 95 ± 2 nM illustrated significant anticancer activity. Apoptotic cells were also studied by acridine orange/ethidium bromide (AO/EB) staining introducing the CPA-Hg(II) complex as a good agent to enhance apoptosis in MDA-MB-231 cell lines. Finally, the biological assays performed in this study show that CPA and its complexes exhibit a higher inhibition of cancer compared with chitosan, especially the CPA-Hg(II) and CPA-Cu(II) complexes.
{"title":"Synthesis and biological assay of biopolymeric chitosan functionalized by phosphoramidic segment P(O)[NH-3Py]2 and its Cu(II), Ni(II) and Hg(II) complexes","authors":"Zeinab Albobaledi ,&nbsp;Atekeh Tarahhomi ,&nbsp;Ali Khaleghian ,&nbsp;Negar Sarmadi","doi":"10.1016/j.ica.2025.122593","DOIUrl":"10.1016/j.ica.2025.122593","url":null,"abstract":"<div><div>Biopolymeric chitosan-phosphoramide (CPA) and its complexes of Cu(II), Ni(II) and Hg(II) were synthesized and characterized by techniques of FT-IR, elemental analysis (CHN), thermogravimetric analysis (TGA), powder X-ray diffraction (PXRD) and scanning electron microscope (SEM). The cytotoxicity of these compounds against breast MDA-MB-231 cell lines was assessed by MTT assay, where the CPA-Hg(II) complex with an IC50 of 95 ± 2 nM illustrated significant anticancer activity. Apoptotic cells were also studied by acridine orange/ethidium bromide (AO/EB) staining introducing the CPA-Hg(II) complex as a good agent to enhance apoptosis in MDA-MB-231 cell lines. Finally, the biological assays performed in this study show that CPA and its complexes exhibit a higher inhibition of cancer compared with chitosan, especially the CPA-Hg(II) and CPA-Cu(II) complexes.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122593"},"PeriodicalIF":2.7,"publicationDate":"2025-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143446069","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}
引用次数: 0
A two-dimensional mixed ligands based coordination polymer of cadmium: Synthesis, single crystal structure and luminescence quenching based sensing behaviors towards Fe3+, Cr3+, Al3+ ions and TNP in aqueous phase
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-13 DOI: 10.1016/j.ica.2025.122592
Priyanka Manna, Akash Kumar Chandra, Partha Mahata
A new Cd (II)-based compound [Cd(BTCH)(L)] (BTCH = di-anionic 1,3,5-benzene tricarboxylic acid and L = 2,4,5-tri-4-pyridyl-1H-imidazole), 1, has been synthesized by hydrothermal method. The structure determined by single-crystal X-ray diffraction revealed two dimensional extended assemblies based on connectivity of Cd2+ ions with two ligands. The presence of one free carboxylic acid groups of each BTCH ligand and one non-bonded pyridine ring of each L ligand makes the two-dimensional layer structure stabilized through the hydrogen bond interactions. The compound has been characterized by powder X-ray diffraction, Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA). Aqueous dispersion of compound 1 showed emission at 400 nm upon excitation at 300 nm. The compound 1 also exhibited photoluminescence-based sensing behaviors towards Fe3+, Al3+ and Cr3+ ions in aqueous medium based on luminescence quenching effect. However, photoluminescence studies in presence of other common metal ions showed either negligible quenching effect or moderate to low turn on effect for Ni2+, K+, Zn2+, Cd2+ Cu2+, Ca2+, Mn2+, Na+, Co2+, Fe2+, Pb2+, Mg2+ in aqueous. The limit of detection for Fe3+, Al3+, Cr3+ ions are 0.568 μM, 1.721 μM and 0.840 μM respectively. Compound 1 also showed significant quenching effect in the presence of 2,4,6-trinitrophenol (TNP) with detection limit of 0.302 μM.
{"title":"A two-dimensional mixed ligands based coordination polymer of cadmium: Synthesis, single crystal structure and luminescence quenching based sensing behaviors towards Fe3+, Cr3+, Al3+ ions and TNP in aqueous phase","authors":"Priyanka Manna,&nbsp;Akash Kumar Chandra,&nbsp;Partha Mahata","doi":"10.1016/j.ica.2025.122592","DOIUrl":"10.1016/j.ica.2025.122592","url":null,"abstract":"<div><div>A new Cd (II)-based compound [Cd(BTCH)(L)] (BTCH = di-anionic 1,3,5-benzene tricarboxylic acid and L = 2,4,5-tri-4-pyridyl-1H-imidazole), <strong>1</strong>, has been synthesized by hydrothermal method. The structure determined by single-crystal X-ray diffraction revealed two dimensional extended assemblies based on connectivity of Cd<sup>2+</sup> ions with two ligands. The presence of one free carboxylic acid groups of each BTCH ligand and one non-bonded pyridine ring of each L ligand makes the two-dimensional layer structure stabilized through the hydrogen bond interactions. The compound has been characterized by powder X-ray diffraction, Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA). Aqueous dispersion of compound <strong>1</strong> showed emission at 400 nm upon excitation at 300 nm. The compound <strong>1</strong> also exhibited photoluminescence-based sensing behaviors towards Fe<sup>3+</sup>, Al<sup>3+</sup> and Cr<sup>3+</sup> ions in aqueous medium based on luminescence quenching effect. However, photoluminescence studies in presence of other common metal ions showed either negligible quenching effect or moderate to low turn on effect for Ni<sup>2+</sup>, K<sup>+</sup>, Zn<sup>2+</sup>, Cd<sup>2+</sup> Cu<sup>2+</sup>, Ca<sup>2+</sup>, Mn<sup>2+</sup>, Na<sup>+</sup>, Co<sup>2+</sup>, Fe<sup>2+</sup>, Pb<sup>2+</sup>, Mg<sup>2+</sup> in aqueous. The limit of detection for Fe<sup>3+</sup>, Al<sup>3+</sup>, Cr<sup>3+</sup> ions are 0.568 μM, 1.721 μM and 0.840 μM respectively. Compound <strong>1</strong> also showed significant quenching effect in the presence of 2,4,6-trinitrophenol (TNP) with detection limit of 0.302 μM.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"580 ","pages":"Article 122592"},"PeriodicalIF":2.7,"publicationDate":"2025-02-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143454268","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}
引用次数: 0
Improving the hydrolase-like activity of a lanthanum(III) complex through second coordination sphere
IF 2.7 3区 化学 Q2 CHEMISTRY, INORGANIC & NUCLEAR Pub Date : 2025-02-11 DOI: 10.1016/j.ica.2025.122588
Carlos A. Lucecki , Daniele C. Durigon , Hernán Terenzi , Adailton J. Bortoluzzi , Ademir Neves , Rosely A. Peralta
In this study, we present a new La(III) complex (2) that demonstrates the ability to catalyze the hydrolysis of 2,4-bis(dinitrophenyl)phosphate (2,4–BDNPP), 2,4-dinitrophenylphosphate (2,4–DNPP), and plasmid DNA. By modulating the second coordination sphere in 2, we were able to independently monitor both mono- and diester hydrolysis. Kinetic studies revealed a 7-fold enhancement in the diesterase performance of 2 relatives to the bare complex (1) and ca 30,000 times the uncatalyzed reaction. Data also indicate that 2 dissociates in solution to yield a binuclear complex, which possesses superior activity compared to its mononuclear counterpart. Finally, DNA assays further confirmed a high cleavage rate promoted by the catalyst. Electrospray ionization mass spectrometry (ESI–MS), potentiometric titration, and kinetic studies were instrumental in identifying catalytically active species and proposing reaction mechanisms.
{"title":"Improving the hydrolase-like activity of a lanthanum(III) complex through second coordination sphere","authors":"Carlos A. Lucecki ,&nbsp;Daniele C. Durigon ,&nbsp;Hernán Terenzi ,&nbsp;Adailton J. Bortoluzzi ,&nbsp;Ademir Neves ,&nbsp;Rosely A. Peralta","doi":"10.1016/j.ica.2025.122588","DOIUrl":"10.1016/j.ica.2025.122588","url":null,"abstract":"<div><div>In this study, we present a new La(III) complex (<strong>2</strong>) that demonstrates the ability to catalyze the hydrolysis of 2,4-bis(dinitrophenyl)phosphate (2,4–BDNPP), 2,4-dinitrophenylphosphate (2,4–DNPP), and plasmid DNA. By modulating the second coordination sphere in <strong>2</strong>, we were able to independently monitor both mono- and diester hydrolysis. Kinetic studies revealed a 7-fold enhancement in the diesterase performance of <strong>2</strong> relatives to the bare complex (<strong>1</strong>) and ca 30,000 times the uncatalyzed reaction. Data also indicate that <strong>2</strong> dissociates in solution to yield a binuclear complex, which possesses superior activity compared to its mononuclear counterpart. Finally, DNA assays further confirmed a high cleavage rate promoted by the catalyst. Electrospray ionization mass spectrometry (ESI–MS), potentiometric titration, and kinetic studies were instrumental in identifying catalytically active species and proposing reaction mechanisms.</div></div>","PeriodicalId":13599,"journal":{"name":"Inorganica Chimica Acta","volume":"579 ","pages":"Article 122588"},"PeriodicalIF":2.7,"publicationDate":"2025-02-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143421896","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}
引用次数: 0
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Inorganica Chimica Acta
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