Powder Diffraction Research Articles

Synthesis of Trimanganese Tetraoxide (Mn3O4) as a promising electrode and Photocatalyst for the degradation of Rhodamine B dye

The article involves the facile bio-synthesis of Manganese (III) Oxide (Mn3O4) nanoparticles (NPs) using Curry leaf (Murraya Koenigii) extract as an efficacious chelating agent. The prepared NPs were subjected to various characterization methods such as Powder X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) with Energy Dispersive X-Ray (EDX) Analysis, Transmission Electron Microscopy (TEM), Fourier Transform Infrared analysis (FTIR), Ultra Violet spectroscopy study (UV–Vis), Cyclic Voltammetry (CV) and Vibrating Sample Magnetometer (VSM) to study the crystalline structure, morphology, optical properties, electrochemical activity and magnetic property of the sample. The XRD result proved the crystallinity of the sample having crystallite size around 15 nm with tetragonal structure. The absorption band observed at 612 cm−1 indicates the Mn-O stretching modes of tetrahedral sites in FTIR analysis of the prepared sample which confirmed the formation of Mn3O4 NPs. Using SEM and TEM techniques, the surface morphology and NPs size were examined. The composition and distribution of the NPs was verified using EDX spectrum and elemental mapping. Using the UV–Visible spectroscopy, the energy band gap (Eg) for the NPs was computed and calculated as 2.34 eV. The Mn3O4 NPs evinced a specific capacitance of 276 Fg-1 at 10 mV/s scan rate. This result proposes that the obtained Mn3O4 NPs can be used as a suitable electrode mainly for supercapacitor applications. VSM study revealed the paramagnetic behavior of the synthesized Mn3O4 NPs. The synthesized Mn3O4 NPs exhibited moderate antibacterial activity with gram positive bacteria such as Staphylococcus aureus, Streptococcus pneumoniae, and gram negative bacteria such as Klebsiella pneumoniae, with the inhibition zones of 12, 10, and 9 mm respectively. Photo catalytic degradation study was carried out for Rhodamine B (RhB) dye, which showed a strong characteristic absorption peak nearly at 554 nm with 94 % of degradation efficiency.

Raman spectroscopic insights into the pressure-induced phase transition in natural elbaite

Tourmaline [XY₃Z₆(T₆O₁₈)(BO₃)₃V₃W] is a potential carrier for water and boron cycles in the Earth's interior. Its high-pressure structural behavior has been extensively investigated by single-crystal or powder X-ray diffraction. Here, we collected Raman spectroscopy data of natural elbaite with two different compositions (Fe-poor elbaite and Fe-rich elbaite) up to 35.1 GPa to complementarily characterize the structural modifications proposed by previous studies. Our results reveal two clear discontinuous changes in high-pressure Raman spectra of both samples. The first change occurred at around 15 GPa, characterized by changes in Raman peak intensity, and the pressure dependence of the frequencies of several lattice vibration modes and hydroxyl stretching vibrations. The second change emerged at around 26 GPa and was marked by the systematic appearance of new Raman peaks. Based on previous X-ray diffraction studies, the change at around 26 GPa is likely caused by a phase transition from rhombohedral R3m to rhombohedral R3, whereas the change at around 15 GPa is likely caused by a change in compression mechanism. Furthermore, the WOH stretching vibrations at 3691 cm−1 in Fe-rich elbaite exhibited a negative pressure coefficient, contrasting with the positive pressure coefficient observed in Fe-poor elbaite, suggesting a significant influence of chemical composition on the evolution of stretching vibration in WOH groups under high pressure. After release of pressure, the spectra return to their initial state, indicating the reversibility of all observed changes.

Determination of the average crystallite size and the crystallite size distribution: the envelope function approach EnvACS

A procedure is presented to exactly obtain the apparent average crystallite size (ACS) of powder samples using standard in-house powder diffraction experiments without any restriction originating from the Scherrer equation. Additionally, the crystallite size distribution within the sample can be evaluated. To achieve this, powder diffractograms are background corrected and long-range radial distribution functions G(r) up to 300 nm are calculated from the diffraction data. The envelope function f env of G(r) is approximated by a procedure determining the absolute maxima of G(r) in a certain interval (r range). Fitting of an ACS distribution envelope function to this approximation gives the ACS and its distribution. The method is tested on diffractograms of LaB6 standard reference materials measured with different wavelengths to demonstrate the validity of the approach and to clarify the influence of the wavelength used. The latter results in a general description of the maximum observable average crystallite size, which depends on the instrument and wavelength used. The crystallite site distribution is compared with particle size distributions based on transmission electron microscopy investigations, providing an approximation of the average number of crystallites per particle.

A red-emitting phosphor Na3AlF6:Mn4+: Green synthesis, optical characteristics, thermal stability and application in high-performance warm WLED

Mn4+-doped fluoride red phosphors have been widely used in warm WLEDs, but the preparation of such phosphor requires the use of a large amount of HF as a fluorine source and an acidic environment. How to reduce the excessive use of highly toxic HF in the preparation process and achieve green synthesis has become a hot research topic. Therefore, a simple green synthesis strategy is proposed in this work to synthesize a series of red-emitting phosphors Na3AlF6:Mn4+. The highly toxic HF solution is replaced by using a low toxicity reaction system (HCl/HNO3 + NH4F), which reduces the direct use of HF. X-ray powder diffraction, energy-dispersive X-ray spectrometer and scanning electron microscope are employed to determine the crystal structure, composition and morphology of all samples. Optical properties are characterized using excitation spectra, emission spectra and fluorescence lifetime curves. The calculation results indicate that the red-light has low correlated color temperature and the excellent color purity, and Na3AlF6 host can provide a strong crystal field environment for Mn4+. In addition, different aluminum sources and Mn4+ doping concentrations are used to explore the optimal preparation condition. The mechanisms of concentration quenching and thermal quenching have also been systematically explored. The stabilities of red-light emission intensity and color are investigated under the high temperature. The integral PL intensity at 423 K is 47 % of the initial value at 298 K. The activation energy, the chromaticity shift and the chromaticity coordinate variation are also systematically calculated. More importantly, a high-performance warm WLED with low correlated color temperature (CCT = 3296 K) and high color rendering index (Ra = 94.7) is achieved by using Na3AlF6:Mn4+ as a red-emitting material. Not only that, the warm WLED exhibits strong output stability under high driving current. The discovery of this work provides a comprehensive understanding for the rational design of high-performance Mn4+-activated fluoride red phosphors via a simple green synthesis strategy.

Formation of Fully Stoichiometric, Oxidation-State Pure Neptunium and Plutonium Dioxides from Molecular Precursors.

Amidate-based ligands (N-(tert-butyl)isobutyramide, ITA) bind κ2 to form homoleptic, 8-coordinate complexes with tetravalent 237Np (Np(ITA)4, 1-Np) and 242Pu (Pu(ITA)4, 1-Pu). These compounds complete an isostructural series from Th, U-Pu and allow for the direct comparison between many of the early actinides with stable tetravalent oxidation states by nuclear magnetic resonance (NMR) spectroscopy and single crystal X-ray diffraction (SCXRD). The molecular precursors are subjected to controlled thermolysis under mild conditions with the exclusion of exogenous air and moisture, facilitating the removal of the volatile organic ligands and ligand byproducts. The preformed metal-oxygen bond in the precursor, as well as the metal oxidation state, are maintained through the decomposition, forming fully stoichiometric, oxidation-state pure NpO2 and PuO2. Powder X-ray diffraction (PXRD), scanning transmission electron microscopy (STEM), and energy dispersive X-ray spectroscopy (EDS) elemental mapping supported the evaluation of these high-purity materials. This chemistry is applicable to a wide range of metals, including actinides, with accessible tetravalent oxidation states, and provides a consistent route to analytical standards of importance to the field of nuclear nonproliferation, forensics, and fundamental studies.

Accelerated Lanthanide Intercalation into Graphite Catalyzed by Na.

Lanthanides (Ln) are notoriously difficult to intercalate into graphite. We investigated the possibility of using Na to catalyze the formation of Ln-intercalated graphite and successfully synthesized LnC6 (Ln = Sm, Eu, and Yb) significantly rapidly in high yields. The synthesis process involves the formation of the reaction intermediate NaCx, through the mixing of Na and C, which subsequently reacts with Ln upon heating to form LnC6. Well-sintered LnC6 pellets with low residual Na concentrations (Ln:Na ≈ 98:2) were fabricated by the two-step method. The pellets enabled the evaluation of LnC6 by powder X-ray diffraction and electrical resistivity measurements. This study highlights the versatility of the Na-catalyzed method and lays the foundation for the rapid mass production of LnC6, with potential applications in superconducting and rechargeable battery materials.

Observation of Haldane magnetism in organically templated vanadium phosphate (enH2)0.5VPO4OH.

We prepared an organically templated magnet, (enH2)0.5VPO4OH (enH2 = diprotonated ethylenediamine), hydrothermally and characterized its crystal structure by powder X-ray diffraction and Fourier-transform infrared spectroscopy, and its physical properties by magnetization, specific heat and nuclear magnetic resonance measurements and density functional theory calculations. (enH2)0.5VPO4OH consists of uniform chains of V3+ (d2, S = 1) ions and exhibits Haldane magnetism with spin gap Δ = 59.3 K from the magnetic susceptibility χ(T) at μ0H = 0.1 T, which is reduced to 48.4 K at μ0H = 9 T according to the 31P shift. The NMR data evidence the formation of a spin-glass state of unpaired S = 1/2 spins at TS-G ≈ 3 K and indicate that the Haldane S = 1 spin chain segments are much longer in the organically templated magnet (enH2)0.5VPO4OH than in the ammonium counterpart NH4VPO4OH. The single-ion anisotropy D and the interchain exchange J' in (enH2)0.5VPO4OH and NH4VPO4OH were estimated in density functional calculations to find them very weak compared to the intrachain exchange J.

Perovskite-Like Carbodiimides AB(NCN)3: Synthesis and Characterization of MnHf(NCN)3 and FeHf(NCN)3.

Two novel ternary air-stable transition-metal carbodiimides, MnHf(NCN)3 and FeHf(NCN)3, were synthesized via solid-state metathesis using either ZnNCN or Na2NCN as the carbodiimide source and the corresponding binary metal chlorides. These two phases are the first examples of transition-metal carbodiimides with an AB(NCN)3 composition, akin to ubiquitous ABO3 perovskite oxides. The crystal structure of MnHf(NCN)3 was determined and refined from powder X-ray diffraction (XRD) data in the non-centrosymmetric space group P6322 allowing for chirality, the assignment of which is supported by second-harmonic generation (SHG) measurements. FeHf(NCN)3 was found to crystallize isotypically, and the presence of iron(II) in a high spin state was confirmed by 57Fe Mößbauer spectroscopy. The structures are revealed to be NiAs-derived and can be described as a hexagonal stack of NCN2- anions with metal cations occupying 2/3 of the octahedral voids. Both IR spectroscopic measurements and DFT calculations agree that the NCN2- unit is a bent carbodiimide with C2v symmetry, necessary to account for the size difference present in such a vacancy-ordered structure. Magnetic studies reveal predominantly strong antiferromagnetic interactions but no long-range order between the paramagnetic Mn2+ centers, likely due to the dilution of Mn2+ over the octahedral sites or perhaps even due to some degree of magnetic frustration. The optical and electrochemical properties of MnHf(NCN)3 were then studied, revealing a wide band gap of 3.04 eV and p-type behavior.

Investigation of the crystal structure, spectral properties, and interactions of N-(R-nitrophenylsulfonamido)benzoic acids with human serum albumin

This study introduced the synthesis of two novel compounds in the N-(R-nitrophenylsulfonamido)benzoic acids (NO2-SBA), designated as HL6 and HL8. Detailed structural information for HL6 and HL8 was acquired through the employment of various characterization techniques such as single-crystal and powder X-ray diffraction, FT-IR spectroscopy, 1H and 13C NMR spectroscopy, and elemental analysis. X-ray diffraction and Hirshfield surface analysis provides a comparative analysis of hydrogen bonding in HL6·H2O and HL8, revealing significant differences in their interaction patterns and resulting crystal structures. Although both molecules possess the same number of hydrogen bond donors and acceptors, the nature of these interactions and their orientations lead to distinct packing arrangements. In HL6·H₂O, the presence of water molecules introduces additional hydrogen bonding possibilities, which are absent in HL8, significantly affecting the overall structure. Additionally, interactions of all nine compounds in the NO2-SBA series [categorized as o-ABA: HL1–HL3, m-ABA: HL4–HL6, and p-ABA: HL7–HL9] with human serum albumin (HSA) were investigated to understand how structural characteristics influence binding mechanisms and affinity. Fluorescence spectroscopy was employed to further examine these interactions, providing a better understanding of their pharmacological properties. The compounds exhibited moderate affinity to HSA, with the o-ABA series displaying a binding constant (Kb) ten times stronger than the other series, underscoring the significant role of the N,R groups in binding interactions.

Probing Defects in Covalent Organic Frameworks.

Defects in covalent organic frameworks (COFs) play a pivotal role in determining their properties and performance, significantly influencing interactions with adsorbates, guest molecules, and substrates as well as affecting charge carrier dynamics and light absorption characteristics. The present review focuses on the diverse array of techniques employed for characterizing and quantifying defects in COFs, addressing a critical need in the field of materials science. As will be discussed in this review, there are basically two types of defects referring either to missing organic moieties leaving free binding groups in the material or structural imperfections resulting in lower crystallinity, grain boundary defects, and incomplete stacking. The review summarizes an in-depth analysis of state-of-the-art characterization techniques, elucidating their specific strengths and limitations for each defect type. Key techniques examined in this review include powder X-ray diffraction (PXRD), infrared spectroscopy (IR), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), scanning transmission electron microscopy (STEM), scanning tunneling microscope (STM), high resolution transmission electron microcoe (HRTEM), gas adsorption, acid-base titration, advanced electron microscopy methods, and computational calculations. We critically assess the capability of each technique to provide qualitative and quantitative information about COF defects, offering insights into their complementary nature and potential for synergistic use. The last section summarizes the main concepts of the review and provides perspectives for future development to overcome the existing challenges.

Impact of Gd doping on structural and magnetic characteristics of SrFeO3 perovskite nanomaterial.

The SrFeO3 nanoparticles doped with 5% and 10% Gd were synthesized using the solution combustion method. The phase formation of the synthesized nanoparticles was confirmed by powder XRD analysis. FESEM and HRTEM were employed to examine the morphology of the samples, revealing well-ordered, agglomerated nanoparticles. EDAX analysis was conducted on all samples, confirming the presence of the desired elements. X-ray photoelectron spectroscopy confirmed the presence of mixed oxidation states of Fe3+ and Fe4+. Magnetization studies, performed using a SQUID magnetometer, showed ferromagnetic behaviour in all samples, with a significant increase in magnetic moment observed with higher Gd doping. The enhanced magnetic moments and reduced coercivity in Gd-doped SrFeO3 suggest that these materials could be suitable for spintronic applications.

Investigation of effect of complexing agent and processing method on solubility of Efonidipine

Nanosponges are versatile carriers due to their exceptional capability to improve the solubility of poorly water-soluble drugs, taste masking and enhancement of stability. This study investigates potential of nanosponges, prepared by crosslinking β-cyclodextrin with diphenyl carbonate in 1:4 ratio for enhancing solubility of Efonidipine. Nanosponges were characterized in terms of particle size. Phase solubility studies and solution state interaction studies were employed to understand the nature and strength of drug: nanosponge complexation. Complexes were prepared by kneading method and spray drying. Saturation solubility, in vitro dissolution studies and molecular modeling studies were performed. Complexes were characterized by differential scanning calorimetry (DSC), infrared spectroscopy, X ray powder diffraction (XRPD) and scanning electron microscopy. Phase solubility studies revealed 1:2 complexation between drug and carriers. Saturation solubility studies showed significant solubility increase with both beta CD and nanosponges. The increase was higher in case of spray dried complexes in all media. An 18 fold increase was observed in case of spray dried complexes in distilled water. DSC and PXRD confirmed amorphization of drug in the complexes. Thus solubility enhancement of EFD could be attributed to complexation and amorphization. Molecular modeling studies revealed the mode of entrapment of efonidipine in the carriers. In conclusion the versatility of nanosponges in encapsulating both hydrophilic and hydrophobic drug molecules holds immense promise for personalized medicine and targeted therapy, ultimately leading to improved patient outcomes. Moreover, the study introduces the efficacy of spray drying as a scalable and practical approach to maximize the solubility-enhancing benefits of nanosponges. This research highlights the potential of nanosponges to overcome a fundamental challenge in pharmaceuticals, opening new avenues for drug delivery and therapeutic advancement. Keywords: Nanosponges, β -cyclodextrin, inclusion complexes, solubility enhancement, molecular modelling

Two Novel Hydrate Salts of Norfloxacin with Phenolic Acids and Their Physicochemical Properties

Norfloxacin (NORF) is a broad-spectrum quinolone that is widely utilized for the treatment of various bacterial infections and is considered one of the most commonly used fluoroquinolone antibiotics. However, NORF’s clinical utility is limited by its poor water solubility and relatively low oral bioavailability. This study presents an optimization and synergistic enhancement approach through salt/co-crystal, aiming to maximize the biopharmaceutical properties of NORF with the use of phenolic acid. Following this strategy, two new hydrate salts of NORF with phenolic acid, namely, NORF—3,5-DBA hydrate (salt 1) and NORF—VA hydrate (salt 2), were prepared and systematically confirmed. Two hydrate salts were produced by means of the slow evaporation crystallization method, and the structures were determined through single-crystal X-ray diffraction (SCXRD). Additionally, powder X-ray diffraction (PXRD), Fourier-transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and high-performance liquid chromatography (HPLC) were applied to analyze the features of the two salts. The experimental results indicated that the formation of the two salts could enhance the solubility and improve the release behavior of NORF. Interestingly, the physicochemical properties of NORF were significantly improved as a result, leading to an enhancement in its antibacterial activity. This was demonstrated by the enhanced inhibition of bacterial strains and the lower minimum inhibitory concentration values.

Crystal structure and tautomeric state of Pigment Red 48:2 from X-ray powder diffraction and solid-state NMR

Crystal structure and tautomeric state of Pigment Red 48:2 from X-ray powder diffraction and solid-state NMR

Correlation between preparation techniques and frictional properties of cellulose nanocrystals as additives in water-based lubricants

To explore the tribological characteristics of cellulose nanocrystals derived through various preparation techniques when utilized as additives in water-based lubricants, two types of cellulose nanocrystals (S-CNC and C-CNC) were chosen. These were produced via sulfuric acid hydrolysis and oxidation methods. The morphology and structural features were assessed through techniques such as Fourier-transform infrared spectroscopy (FT-IR), X-ray powder diffraction (XRD), laser confocal Raman spectroscopy, elemental analysis, scanning electron microscopy (SEM), and laser particle size analysis. According to thermogravimetric analysis (TGA), the thermal stability of S-CNC is slightly superior to that of C-CNC. S-CNC exhibits liquid crystallinity when the concentration exceeds 0.5 %, whereas C-CNC does not display liquid crystallinity at any concentration tested. Further investigation was conducted on the frictional properties of the two types of CNCs using a UMT reciprocating friction tester. The results indicate that both types of CNC exhibit significant friction reduction properties at various additive concentrations, provided the addition does not exceed w=1 %. When below their respective liquid crystalline phase concentrations, the friction reduction performance of S-CNC is slightly inferior to that of C-CNC; however, when above the liquid crystalline phase concentration, the friction reduction performance of S-CNC surpasses that of C-CNC. The addition of w=0.5 % S-CNC leads to a relative reduction of 63.4 % in the friction coefficient compared to the base system. Analysis of the steel plate surface contact angle and post-wear surface suggests that the lubrication mechanism of CNC involves the adsorption of polar functional groups such as hydroxyl or carboxyl groups from the CNC structure onto the friction pair surface, forming a lubricating protective film to varying degrees. Additionally, the liquid crystalline structure of S-CNC facilitates the formation of an ordered lubricating film, further enhancing the frictional properties. These findings provide valuable insights into the application of nanocellulose crystals as lubricant additives.

Assessment and monitoring of leather effluent discharge from Dewas and Ranipet and their computational approach.

The swift pace of industrialization, urbanization, and burgeoning populations propel the surge in demand for manufactured goods and infrastructure. The wastewater produced during leather processing comprises a cocktail of organic and inorganic chemical contaminants that have the potential to affect the environment. This study focuses on conducting a comparative physico-chemical, analytical,in vitro, and in silicotoxicity assessment and monitoring of leather effluent discharged from two different areas, namely, Dewas and Ranipet. The physicochemical analysis of collected effluents revealed higher levels of biochemical oxygen demand, chemical oxygen demand, total dissolved solids, total suspended solids, and heavy metals than the permissible limit fixed by the Central Pollution Control Board (CPCB). The X-ray powder diffraction analysis of both samples identified the existence of crystalline and amorphous phases. The functional composition of compounds was identified through the analysis of Fourier-Transform Infrared Spectroscopy, which revealed the existence of C-H, O-H, N-H, C = O, C=C, and C≡C stretching vibrations. A variety of compound derivatives, including amines, organic acids, organometallic compounds, alcohols, hydrocarbons, esters, aldehydes, ketones, aromatic, and organogermanium, were identified by Gas Chromatography-Mass Spectrometry. An assessment and monitoring of the phytotoxicity of effluent on the germination of Vigna radiata seeds reveals that (100%) of both Dewas and Ranipet leather effluents inhibited seed germination by 33.34% and 100%. The incorporation of Absorption-Distribution-Metabolism-Excretion-Toxicity (ADMET) analysis improved comprehension of the toxicity profiles of the GC-MS-identified compounds. Moreover, the result of docking studies revealed that cytochrome P450 showed the highest binding affinity towards 1,3-benzodioxol-2-one, hexahydro-cis with an affinity score of - 7.1kcal/mol. The overall research revealed that the leather effluents from Dewas and Ranipet exhibit significant toxicity, highlighting the necessity of better wastewater management. In the future, innovative treatment methods and environmental friendly processes can be developed to minimize the detrimental effects of leather effluents.

Dramatic Impact of Materials Combinations on the Chemical Organization of Core-Shell Nanocrystals: Boosting the Tm3+ Emission above 1600 nm.

This article represents the first foray into investigating the consequences of various material combinations on the short-wave infrared (SWIR, 1000-2000 nm) performance of Tm-based core-shell nanocrystals (NCs) above 1600 nm. In total, six different material combinations involving two different types of SWIR-emitting core NCs (α-NaTmF4 and LiTmF4) combined with three different protecting shell materials (α-NaYF4, CaF2, and LiYF4) have been synthesized. All corresponding homo- and heterostructured NCs have been meticulously characterized by powder X-ray diffraction and electron microscopy techniques. The latter revealed that out of the six investigated combinations, only one led to the formation of a true core-shell structure with well-segregated core and shell domains. The direct correlation between the downshifting performance and the spatial localization of Tm3+ ions within the final homo- and heterostructured NCs is established. Interestingly, to achieve the best SWIR performance, the formation of an abrupt interface is not a prerequisite, while the existence of a pure (even thin) protective shell is vital. Remarkably, although all homo- and heterostructured NCs have been synthesized under the exact same experimental conditions, Tm3+ SWIR emission is either fully quenched or highly efficient depending on the type of material combination. The most efficient combination (LiTmF4/LiYF4) achieved a high photoluminescence quantum yield of 39% for SWIR emission above 1600 nm (excitation power density in the range 0.5-3 W/cm2) despite significant intermixing. From now on, highly efficient SWIR-emitting probes with an emission above 1600 nm are within reach to unlock the full potential of in vivo SWIR imaging.

Synthesis, crystal structures, characterizations and antibacterial activities for four lithium(I)-based metal organic frameworks

Lithium(I)-based compounds are extensively utilized across various domains, however, their structural characteristics remain inadequately explored, which has hindered further development and application of their functionalities. Thus, the exploration of their structural intricacies is crucial for unlocking their full potential and paving the way for innovative applications in diverse fields. In this study, four Li(I)-based metal organic frameworks (MOFs), namely, [Li4(BNZ)4(H2O)4]n (1), [Li(HBNZ)]n (2), [Li(BNZ)(DPRO)]n (3), [Li2(MBNZ)2(DPRO)2]n (4), are synthesized through hydrothermal method, and structurally characterized by single crystal X-ray diffraction, powder X-ray diffraction, and IR, where BNZ, HBNZ, MBNZ and DPRO are benzoic acid, 4-hydroxybenzoic acid, 3-methoxybenzoic acid and d-proline, respectively. Crystallographic analysis reveals that all these complexes are two-dimensional layered architectures, of which 3 and 4 display a similar wave-like square grids network. The crystal structures of the complexes 1–4 are stabilized by one or more kinds of NH···O, CH···O, OH···O, CH···π, π-π interactions, and the intermolecular interactions and thermal stabilities of these complexes were also analyzed by Hirshfeld surface and thermogravimetric analysis, respectively. Moreover, these complexes show the great photoluminescence properties and antibacterial activities, exhibiting remarkable potential applications in both material and pharmaceutical science, and the necessity for continued research to promise a paradigm shift in the design and application of advanced materials.

Pyrazolone-Based Zn(II) Complexes Display Antitumor Effects in Mutant p53-Carrying Cancer Cells.

The synthesis and characterization of nine Schiff bases of pyrazolone ligands HLn (n = 1-9) and the corresponding zinc(II) complexes 1-9 of composition [Zn(Ln)2] (n = 1-9) are reported. The molecular structures of complexes 2, 3, 4, 8, and 9 were determined by single-crystal X-ray diffraction analysis, highlighting in all cases a distorted tetrahedral geometry around the Zn(II) ion. Density functional theory studies are performed on both the HLn ligands and the derived complexes. A mechanism of dissociation and hydrolyzation of the coordinated Schiff base ligands is suggested, confirmed experimentally by powder X-ray diffraction study and photophysical studies. Complexes 1-9 were investigated in vitro as anticancer agents, along with mutant p53 (mutp53) protein levels in human cancer cell lines carrying R175H and R273H mutp53 proteins. Only those complexes with the highest Zn(II) ion release via dissociation have shown a significant cytotoxic activity with reduction of mutp53 protein levels.

Enhanced ion separation by amine grafted graphene oxide-tripolyphosphate anionic composite membrane based on polyvinylidene fluoride

The amine functionalized graphene oxide (GO) was prepared via a chemical reaction. This was achieved by reacting GO with a mixture of ethanolamine, N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride, and sodium tripolyphosphate (STTP). The amine-functionalized graphene oxide (EGOS) with varying STTP:GO weight ratios was then used to fabricate cation-exchange membranes (CEMs) based on polyvinylidene fluoride. The characterizations of the modified EGOS samples were investigated using various techniques, such as Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), Raman spectroscopy, and energy dispersive spectroscopy (EDS). Furthermore, the influence of the STTP:GO weight ratio in the EGOS samples on the properties of the fabricated CEMs was investigated using different experimental methods. More desirable characteristics were recorded for the EGOS-based CEMs compared to GO-containing membranes. The top-performance membrane comprising EGOS0.5 (STTP: GO weight ratio of 0.5:1) demonstrated a remarkable water content of 45.6 ± 1.3 %, and an ion exchange capacity of 3.6 ± 0.3 meq g−1. The electrochemical impedance spectroscopy results showed that this membrane has the lowest resistance of 1.5 Ω cm2, which was considerably (86.96 %) less than the value obtained for the unmodified GO-containing reference membrane (11.5 Ω cm2). The diffusion coefficient of sodium ions through the fabricated CEMs was investigated via electrochemical cyclic voltammetry (CV) and the Randles-Sevceks equation and the highest value was obtained for EGOS0.5-based CEMs.