X-ray Studies Research Articles

Photoluminescence and supercapacitor applications of dysprosium doped rhombohedral silver gallium oxide nanoparticles

Dy3+ doped Silver Gallium Oxide (AgGaO2) nanoparticles (NPs) (AGO:Dy3+) are effectively synthesized via a green mediated route using Aloe vera gel extract as a reducing agent, followed by calcination at 600 °C for 3 h. Powder X-ray diffraction (PXRD), Fourier transformation infrared (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), photoluminescence (PL), and electrochemical studies were employed to confirm the synthesis, structural, luminescence, and supercapacitor properties of the NPs. The diffraction peaks of the synthesized samples possess a trigonal structure within a rhombohedral system. The surface morphology consists of a few irregular, a few hexagonal, and a few rice grain-structured NPs. The changes in the agglomeration were observed with variations in the dopant concentration. The direct energy band gap increases from 3.11 to 3.13 eV with an increase in the dopant concentration. Under 276 nm excitation, the PL spectra of AGO:Dy3+ nanophosphors reveal robust emission peaks attributed to 4F9/2→6F15/2 (480 nm) and 4F9/2→6F13/2 (565 nm). The confirmed critical distance signifies that energy transfer occurs through a multipolar interaction mechanism. The CIE chromaticity diagram illustrates the emission of yellowish green light from the phosphors. These investigations indicate the potential applications of AGO:Dy3+ nanocrystals in a light-emitting diode as a nanophosphor material. Nanocrystals in light-emitting diodes as a nanophosphor material. Thorough electrochemical investigations, encompassing cyclic voltammetry, were conducted to decipher redox reactions, electrode kinetics, and electrochemical behavior. The precise elucidation of ion transport kinetics was achieved through Electrochemical Impedance Spectroscopy (EIS), while the determination of supercapacitance values was accomplished via Galvanostatic Charge-Discharge (GCD) analysis. The supercapacitance values exhibited a remarkable range from 76.177 to 111.53 F/g, underscoring their sensitivity to dopant concentration. Consequently, the material synthesized in this groundbreaking study exhibits substantial promise for diverse applications, spanning from energy storage materials to the dynamic landscape of display technology. Electrochemical studies.

Highly Stable Self-Regenerating Organic Multi-Redox Systems derived from Bicyclic (Alkyl)(amino)carbenes (BICAACs).

An extended class of organic multi-redox systems was derived from bicyclic(alkyl)amino carbenes (BICAACs). The highly-conjugated system undergoes a total of 4 redox events spanning a 1.8 V redox range. These organic compounds exhibited four different stable redox states (dication, radical cation, neutral and radical anion), and all of them were characterized either by single crystal X-ray study and/or various spectroscopic studies. Three of the four redox states are stable to air and moisture. The availability of stable multiple redox states demonstrated promise towards their efficacy in the symmetric H-cell charge/discharge cycling. Among various redox states, the dication/neutral state works efficiently and continuously for 1500 cycles in 2e- charge/discharge process outside glovebox in commercially available DMF with minimum capacity loss (retaining nearly 90 % Coulombic efficiency). Surprisingly, the efficiency of the redox cycle was retained even if the system was exposed to air for 30 days when it slowly regenerated to the initial deep blue radical cation, and it exhibited another 100 charge/discharge cycles with a minimal capacity loss. Such a stable H-cell cycling ability is not well known among organic molecule-based systems.

Stirrer design for improving fluidization of cohesive powder: A time-resolved X-ray study

Stirring has been recognized in the literature as a promising technique for facilitating fluidization of cohesive powders, via inputting additional energy to counteract interparticle forces. However, the influence of operating conditions and stirrer configurations on flow behavior remains largely unknown, which impedes the practical implementation of stirred fluidization. Utilizing X-ray imaging, this research demonstrates that stirring enhances fluidization in cohesive micron-silica powder (Sauter mean diameter ▪) by collapsing the powder packing structure, and transitioning channeling beds into bubbling states. Comb-like configurations featuring fewer stirrers and blades, placed in the bottom region, have shown to be highly effective. Excessive stirring can lead to air pockets and a compacted phase of particles on the column walls, undermining the interaction between particles and stirrers. Additionally, the experiments show that maximizing the sweeping coverage, employing complex asymmetrical configurations, and avoiding tortuous gas pathways are preferable.

An X-Ray Census of Active Galactic Nuclei in the Virgo and Fornax Clusters of Galaxies with SRG/eROSITA

We present a uniform and sensitive X-ray census of active galactic nuclei (AGNs) in the two nearest galaxy clusters, Virgo and Fornax, utilizing the newly released X-ray source catalogs from the first all-sky scan of Spectrum-Roentgen-Gamma/eROSITA. A total of 50 and 10 X-ray sources are found positionally coincident with the nuclei of member galaxies in Virgo and Fornax, respectively, down to a 0.2–2.3 keV luminosity of ∼1039 erg s−1 and reaching out to a projected distance well beyond the virial radius of both clusters. The majority of the nuclear X-ray sources are newly identified. There is weak evidence that the nuclear X-ray sources are preferentially found in late-type hosts. Several hosts are dwarf galaxies with a stellar mass below ∼109 M ⊙. We find that contamination by nonnuclear X-ray emission can be neglected in most cases, indicating the dominance of a genuine AGN. In the meantime, no nuclear X-ray source exhibits a luminosity higher than a few times 1041 erg s−1, which might be owing to a steep intrinsic luminosity function. The X-ray AGN occupation rate is only ∼3% in both clusters, apparently much lower than that in field galaxies inferred from previous X-ray studies. Both aspects suggest that the cluster environment effectively suppresses AGN activity. The findings of this census have important implications for the interplay between galaxies and their central massive black holes in cluster environments.

Comprehensive computational insights on the conformations, electronic properties and binding mechanism of mescaline: A hallucinogenic molecule

In the series of computational investigations of hallucinogenic compounds particularly in unraveling their conformational aspects, mescaline is taken up in this report after having studied psilocybin and psilocin. Six conformers were identified from the relaxed scan of the dihedral angles of which two were taken up for studying their chemical properties. The two low energy conformers differed by about 0.5 kcal.mol-1 at B3LYP/cc-pVTZ and 1.5 kcal.mol-1 at CCSD/cc-PVDZ levels of theory, respectively and structurally the two conformers differ by the orientation of the alkyl amine group vis-à-vis the benzene ring via the N–H---π interaction. Natural Bond Orbital calculations unveiled the existence of intra-molecular π → π*, n → π* charge transfers, and some hyperconjugative interactions that significantly enhance the stability of mescaline. Reduced Density Gradient calculations unraveled the occurrence of strong intramolecular N–H---π interaction in the most stable conformer of mescaline. The calculated geometrical parameters and predicted structure of the most stable conformer of mescaline agree significantly well with the earlier reported conformers from X-ray studies of mescaline. The computed λmax in the UV–visible spectrum, peak positions in the proton NMR spectrum, and vibrational modes exhibit excellent agreement with the previously reported experimental findings. Moreover, we utilized molecular docking and molecular dynamics simulations to elucidate the binding mode and molecular mechanism of mescaline in comparison to other hallucinogenic molecules. Our findings revealed that mescaline displayed a favorable binding energy and induced essential conformational changes, indicating a potential common mechanism of action shared with psilocybin, another hallucinogenic compound.

Operando synchrotron-based X-ray study and intervention approaches of graphene-related-materials for investigating the performance and durability of HT-PEMFC

The application of high-temperature proton exchange membrane fuel cells (HT-PEMFCs) addresses challenges in water management, fuel purity, and overheating under high current density. However, phosphoric acid (PA) migration hinders their development. This study uses synchrotron-based X-ray fluorescence spectroscopy to investigate PA and catalyst migration. Interventions with single-layer graphene and electrochemically exfoliated graphene oxide improve performance and durability. X-ray absorption spectroscopy provides insights into relevant mechanisms, advancing understanding of membrane electrode assembly preparation and the intricate influences of PA and catalyst migration on performance and durability in HT-PEMFCs.

Distraction osteogenesis in combined sequential use of external fixation and nailing (lengthening and then nailing): An experimental study in rabbits.

Limb lengthening relies on the process of distraction osteogenesis. The active periosteal bone formation has been detected in clinical practice with a lengthening and then nail (LATN) technique but has not been confirmed by experimental studies to date. The aim of this study is to compare the tissue regeneration of the distraction regenerate during tibial lengthening in rabbits using a LATN technique. This study was performed on 54 mature rabbits of the Soviet Chinchilla breed, which were divided into three groups of 18 animals. In group 1 (control), the tibia was lengthened in an external fixator. In group 2, the LATN technique was modeled and in group 3, lengthening over nail (LON) was modeled. The total duration of the experiment was 45 days. On the 10th, 15th, 20th, 30th, and 45th day X-ray, computed tomography and morphological studies were performed. In the experimental groups (2 and 3), a more pronounced periosteal bone formation in the area of regenerate was noted when compared to group 1. In group 2 (LATN), wide cortical plates were formed from the intermediate and periosteal areas. In this group, the maximum densitometric density values were noted. Endosteal bone formation was preserved in all groups. The LON and LATN techniques, when compared with the classical Ilizarov lengthening, do not demonstrate any deficiency in the tissue regeneration of the bone tissue at the regenerate sites. The most powerful bone structures are formed with the sequential use of the external fixation and nailing (LATN).

ORTHODONTIC EXTRUSION TECHNIQUE AS A METHOD FOR ALVEOLAR BONE VOLUME INCREASE BEFORE DENTAL IMPLANTATION. CLINICAL CASE

Objectives: Tooth extraction and replacement with dental implant represents a common treatment choice, when teeth are hopeless. We presented a clinical case, the treatment of which was carried out by the method of orthodontic extrusion technique. This technique can increase alveolar bone level and also soft tissue level. The increased amount of alveolar bone can improve primary implant stability and be compared with bone regeneration techniques. The purpose of presenting this clinical case is to emphasize the efficiency of orthodontic extrusion. Methods and materials: A 45-year-old female patient referred by the general dentist regarding cosmetic defect and tooth mobility in the area of the anterior upper teeth. During the examination, her upper right central incisor was found to be mobile, with diastema and slight congestion in the anterior teeth Photographs, CT and X-ray studies of the patient were used. The patient was bonded with .018 slot Roth prescription ceramic brackets (Dentaurum, Germany). After achieving the optimal results of orthodontic treatment and the necessary extrusion of the upper right central incisor, the tooth was removed and replaced with a dental implant. After six months, the patient had a crown with a screw fixation of zirconium dioxide with ceramic application Results: As a result of orthodontic extrusion, clinically significant increase in alveolar bone and gingival tissue was reported. This resulted significant qualitative and quantitative improvements in the implant site. As the clinical case was in aesthetic zone, we could also rehabilitate beautiful smile of patient and increase her self-esteem. Conclusions: Summing up the above and the results of the treatment of this patient, we can definitely say that orthodontic extrusion technique is effective for implant site development. As we have described, this can effectively move the facial gingival margin and allow for esthetic restoration of implant placed in the extruded tooth position without any bone graft.

Intramolecular Cation-π Interactions Organize Bowl-Shaped, Luminescent Molecular Containers.

Molecules with nonplanar architectures are highly desirable due to their unique topological structures and functions. We report here the synthesis of two molecular containers (1 ⋅ 3Br- and 1 ⋅ 3Cl-), which utilize intramolecular cation-π interactions to enforce macrocylic arrangements and exhibit high binding affinity and luminescent properties. Remarkably, the geometry of the cation-π interaction can be flexibly tailored to achieve a precise ring arrangement, irrespective of the angle of the noncovalent bonds. Additionally, the C-H⋅⋅⋅Br- hydrogen bonds within the container are also conducive to stabilizing the bowl-shaped conformation. These bowl-shaped conformations were confirmed both in solution through NMR spectroscopy and in the solid state by X-ray studies. 1 ⋅ 3Br- shows high binding affinity and selectivity: F->Cl-, through C-H⋅⋅⋅X- (X=F, Cl) hydrogen bonds. Additionally, these containers exhibited blue fluorescence in solution and yellow room-temperature phosphorescence (RTP) in the solid state. Our findings illustrate the utility of cation-π interactions in designing functional molecules.

Prospects for the use of computer vision for abdominal CT

Radiology has undergone several significant changes in recent years. Technologies based on computer vision are being actively introduced and allow improving and accelerating the diagnosis of many diseases, as well as reducing the burden on medical personnel. At the same time, these technologies have already proven their effectiveness in routine practice in the analysis of X-ray studies of the mammary glands and chest organs. Also recently, solutions have appeared for the search, qualitative and quantitative evaluation of such common pathologies as urolithiasis and volumetric formations in the parenchyma of the liver and kidneys with a sufficiently high accuracy.
 Currently, there are many different architectures of deep learning networks and computer vision algorithms that allow identifying and classify the pathology of the abdominal organs. At the same time, all models can be divided into algorithms that distinguish (segment) pathology and algorithms that allow classification of the pathology of the abdominal organs.
 This review evaluates the existing computer vision algorithms used in computed tomography of the abdominal organs, determines the main directions of their development, and provides prospects for application in medical organizations.

Synthesis, Characterization, and Biological Studies of Metal Complexes of Dicoumarol Derivatives of Gatifloxacin

Copper(II) complexes were prepared using gatifloxacin and dicoumarin derivatives to investigate their biological activities and to conduct X-ray studies. The complexes were synthesized through classical thermal methods. Biologically potent ligands were synthesized by the reaction of dicoumarin derivative with different aldehydes in ethanol. Cu(II) complexes were formed by mixing ethanolic solution of ligands and gatifloxacin with metal solutions in a 1:1 mole ratio. The structures of the dicoumarin derivatives and their Cu(II) complexes were analyzed by infrared, 1H NMR, 13C NMR, and mass spectrometry. The thermal behavior of the new mixed ligand Cu(II) complexes was investigated by thermogravimetric, fast atom bombardment (FAB) mass, and X-ray analysis. The iron-reducing antioxidant potential (FRAP) (antioxidant activity) of all compounds was evaluated. All the synthesized compounds were screened for antibacterial activity against Escherichia coli; Pseudomonas aeruginosa; Streptococcus pyogenes; minimum inhibitory concentration values for Candida albicans; and Aspergillus niger were determined using the Luria Broth dilution method. The ligands and their complexes were evaluated for antioxidant and antibacterial activity in vitro. The complexes exhibited better results than their respective counterparts.. KEYWORDS :Antimicrobial, Antioxidant, Fast atom bombardment mass, Thermal analysis, Thermo gravimetric analysis, X-ray.

Environmental dependence of AGN activity and star formation in galaxy clusters from Magneticum simulations

Context. The environment inside and on the outskirts of galaxy clusters has a profound impact on the star formation rate and active galactic nucleus (AGN) activity in cluster galaxies. While the overall star formation and AGN suppression in the inner cluster regions has been thoroughly studied in the past, recent X-ray studies also indicate that conditions on the cluster outskirts may promote AGN activity. Aims. We investigate how the environment and the properties of host galaxies impact the levels of AGN activity and star formation in galaxy clusters. We aim to identify significant trends in different galaxy populations and suggest possible explanations. Methods. We studied galaxies with stellar mass log M*(M⊙) > 10.15 in galaxy clusters with mass M500 > 1013 M⊙ extracted from box2b (640 comoving Mpc h−1) of the Magneticum Pathfinder suite of cosmological hydrodynamical simulations at redshifts 0.25 and 0.90. We examined the influence of stellar mass, distance to the nearest neighbouring galaxy, cluster-centric radius, substructure membership, and large-scale surroundings on the fraction of galaxies hosting an AGN, star formation rate, and the ratio between star-forming and quiescent galaxies. Results. We find that in low-mass galaxies, AGN activity and star formation are similarly affected by the environment and decline towards the cluster centre. In massive galaxies, the impact is different; star-formation level increases in the inner regions and peaks between 0.5 and 1 R500 with a rapid decline in the centre, whereas AGN activity declines in the inner regions and rapidly rises below R500 towards the centre. We suggest that this increase is a result of the larger black hole masses relative to stellar masses in the cluster centre. After disentangling the contributions of neighbouring cluster regions, we find an excess of AGN activity in massive galaxies on the cluster outskirts (∼3 R500). We also find that the local density, substructure membership, and stellar mass strongly influence star formation and AGN activity but verify that they cannot fully account for the observed radial trends.

Flux Contribution and Geometry of Charge Exchange Emission in the Starburst Galaxy M82

Recent X-ray studies of starburst galaxies have found that charge exchange (CX) commonly occurs between outflowing hot plasma and cold gas, possibly from swept-up clouds. However, the total CX flux and the regions where CX occurs have been poorly understood. We present an analysis of XMM-Newton observations of M82, a prototype starburst galaxy, aiming to investigate these key properties of CX emission. We have used a blind source separation method in an image analysis of CCD data, which identified a component with the enhanced O–K lines expected from the CX process. Analyzing the XMM-Newton/RGS spectra from the regions identified by the image analysis, we have detected a high forbidden-to-resonance ratio of the O vii Heα triplet as well as several emission lines from K-shell transitions of C, N, and O that are enhanced by the CX process. CX is less responsible for the emission lines of Ne and Mg, and accurate estimation of the CX contribution is confirmed to be crucial in measuring chemical abundances. The temperature of the plasma acting as an electron receiver in the CX process is significantly lower compared to that of the plasma components responsible for most of the X-rays. From the low temperature and an estimation of the CX-emitting volume, we find that the CX primarily occurs in a limited region at interfaces between plasma and gas whose temperatures rapidly decrease due to thermal conduction.

XFEL structure of carbonic anhydrase II: a comparative study of XFEL, NMR, X-ray and neutron structures.

The combination of X-ray free-electron lasers (XFELs) with serial femtosecond crystallography represents cutting-edge technology in structural biology, allowing the study of enzyme reactions and dynamics in real time through the generation of `molecular movies'. This technology combines short and precise high-energy X-ray exposure to a stream of protein microcrystals. Here, the XFEL structure of carbonic anhydrase II, a ubiquitous enzyme responsible for the interconversion of CO2 and bicarbonate, is reported, and is compared with previously reported NMR and synchrotron X-ray and neutron single-crystal structures.

Formulation and Development of Novel Sulfasalazine Bilayer Tablets for The Treatment of Arthritis Associated With IBD: In-vitro and In-vivo Investigations

Sulfasalazine needs frequent daily dosing and the administration of numerous tablets per day pose challenges to patient compliance, contributing to increased adverse effects and difficulties in disease control. These inconveniences result in less effective treatment for arthritis associated with inflammatory bowel disease i.e. ulcerative colitis etc. To improve drug bioavailability, a delayed-release mechanism that releases the drug at the colon is necessary. To develop and optimize colon-targeted controlled release bilayer tablets coated with pH-dependent polymers. The bilayer tablets containing the immediate release part and sustained release part were developed. The tablets were coated with enteric-coated with Eudragit® S-100 and l-100 to achieve release in the colon. Granule properties and tablets were evaluated. The physicochemical parameters of the tablets were evaluated including, stability study, and drug release in 0.1 N HCl (pH 1.2), pH 6.8 phosphate buffer, pH 7.4 phosphate buffer for 2, 1, and up to 24 h respectively. Radiographic imaging and in vivo pharmacokinetic studies were also done in Rabbits. The bilayer tablets containing immediate and sustained release were successfully developed for the colon targeting. The granule properties were found within the acceptable range indicating good flow properties. The physicochemical properties of the tablets were also found acceptable. The tablets did not show release in 0.1 N HCl and 6.8 phosphate buffer but drug release was found under control in the 7.4 pH buffer. Sulfasalazine coated bilayer tablets were found stable and no significant changes were observed in the stability studies. Based on the X-ray studies, the formulated tablet remained discernible in the stomach, small intestine, and colon for a duration of up to 24 h. Finally, by the 32nd hour, the tablet was no longer visible in the X-ray examination, leading to the conclusion of complete drug release. The drug concentration in plasma remained within the therapeutic range for up to 24 h in vivo. These novel formulations present substantial advantages, providing prolonged targeted drug release and reducing systemic adverse effects. The results suggest promising potential for treating arthritis in Inflammatory bowel disease (IBD) patients, offering a solution to current delivery systems.

New examples of ferroelectric nematic materials showing evidence for the antiferroelectric smectic-Z phase

We present a new ferroelectric nematic material, 4-((4′-((trans)-5-ethyloxan-2-yl)-2′,3,5,6′-tetrafluoro-[1,1′-biphenyl]-4-yl)difluoromethoxy)-2,6-difluorobenzonitrile (AUUQU-2-N) and its higher homologues, the molecular structures of which include fluorinated building blocks, an oxane ring, and a terminal cyano group, all contributing to a large molecular dipole moment of about 12.5 D. We observed that AUUQU-2-N has three distinct liquid crystal phases, two of which were found to be polar phases with a spontaneous electric polarization Ps of up to 6 µC cm–2. The highest temperature phase is a common enantiotropic nematic (N) exhibiting only field-induced polarization. The lowest-temperature, monotropic phase proved to be a new example of the ferroelectric nematic phase (NF), evidenced by a single-peak polarization reversal current response, a giant imaginary dielectric permittivity on the order of 103, and the absence of any smectic layer X-ray diffraction peaks. The ordinary nematic phase N and the ferroelectric nematic phase NF are separated by an antiferroelectric liquid crystal phase which has low permittivity and a polarization reversal current exhibiting a characteristic double-peak response. In the polarizing light microscope, this antiferroelectric phase shows characteristic zig-zag defects, evidence of a layered structure. These observations suggest that this is another example of the recently discovered smectic ZA (SmZA) phase, having smectic layers with the molecular director parallel to the layer planes. The diffraction peaks from the smectic layering have not been observed to date but detailed 2D X-ray studies indicate the presence of additional short-range structures including smectic C-type correlations in all three phases—N, SmZA and NF—which may shed new light on the understanding of polar and antipolar order in these phases.

Design of floating formulations and antiulcer activity of Desmostachya bipinnata

The study aims to design and optimize the floating formulations of the aqueous extract of Desmostachya bipinnata (ADB) to treat peptic ulcers. The trial concentrations of HPMC E50, HPMC K4M, and Carbopol 940 were used as factors, and floating lag time, total floating time, and % drug release at 12 h were used as responses. The formulation underwent evaluation for different parameters: aspirin-induced ulcers in rats assessed the antiulcer activity, and X-ray studies in rabbits evaluated the gastroretentive nature. The optimized formulation has shown a floating lag time of 32 s and floated in the gastric medium for more than 9 h with a maximum drug release of 93% at the end of 12 h by following the Korsmeyer-Peppas drug release mechanism. The optimized formulation has good flow properties. The FT-IR, DSC, and XRD studies show ADB and excipients didn't show any incompatibility. The formulation has shown significant antiulcer activity against aspirin-induced ulcers in rats, with an ulcer index of 3.38 ± 0.24 and inhibition of 76.67 ± 0.56%. The in vivo X-ray imaging proved the gastric retention of the formulations for more than 8 h. The results of the formulations demonstrate the floating ability and sustained drug release of the tablet responsible for treating peptic ulcers to show a localized effect in the gastric region and to maintain the ROS levels.Graphical

Control of nano-cavitation in semi-crystalline polymer nanocomposites during uniaxial tension: In situ synchrotron X-ray study

The cavitation behavior of polypropylene-silica (PP-silica) and high density polyethylene-silica (HDPE-silica) composites with varying silica content during uniaxial tension was investigated via in situ X-ray techniques. The introduction of silica was found to significantly influence the mechanical properties of the materials. Small-angle X-ray scattering (SAXS) was employed to determine the cavitation onset strain and to observe the evolution of cavity structures. Through model fitting, the size evolution of nanoscale cavities at the onset of cavitation was quantitatively characterized. Scanning electron microscopy (SEM) was utilized to examine the morphology before and after stretching, revealing that cavity structures primarily resulted from internal defects in the polymer matrix and interfacial debonding between silica and the polymer. The long axis of the nanoscale cavities at the onset of cavitation was perpendicular to the tensile direction, and further deformation led to the coalescence into micron-sized cavities with the long axis parallel to the tensile direction. Wide-angle X-ray scattering (WAXS) was used to characterize the microscale deformation process of crystals, showing that during stretching, the lamellae reoriented with the angle between their normal direction and the tensile direction gradually decreasing. Several sets of transition strains representing the plastic deformation were used to compare the microscale and macroscale deformation, elucidating the sequence and differentiation between crystal plastic deformation, cavitation, and yield in the two polymer materials. Intriguingly, both PP-silica and HDPE-silica composites exhibited optimal silica additions and initial structural parameters for regulating cavitation behavior. These findings offer significant guidance for the control of internal structures in porous separators in industrial production.

Copper interaction with cystatin C: effects on protein structure and oligomerization.

Human cystatin C (hCC), a small secretory protein, has gained attention beyond its classical role as a cysteine protease inhibitor owing to its potential involvement in neurodegenerative disorders. This study investigates the interaction between copper(II) ions [Cu(II)] and hCC, specifically targeting histidine residues known to participate in metal binding. Through various analytical techniques, including mutagenesis, circular dichroism, fluorescence assays, gel filtration chromatography, and electron microscopy, we evaluated the impact of Cu(II) ions on the structure and oligomerization of hCC. The results show that Cu(II) does not influence the secondary and tertiary structure of the studied hCC variants but affects their stability. To explore the Cu(II)-binding site, nuclear magnetic resonance (NMR) and X-ray studies were conducted. NMR experiments revealed notable changes in signal intensities and linewidths within the region 86His-Asp-Gln-Pro-His90, suggesting its involvement in Cu(II) coordination. Both histidine residues from this fragment were found to serve as a primary anchor of Cu(II) in solution, depending on the structural context and the presence of other Cu(II)-binding agents. The presence of Cu(II) led to significant destabilization and altered thermal stability of the wild-type and H90A variant, confirming differentiation between His residues in Cu(II) binding. In conclusion, this study provides valuable insights into the interaction between Cu(II) and hCC, elucidating the impact of copper ions on protein stability and identifying potential Cu(II)-binding residues. Understanding these interactions enhances our knowledge of the role of copper in neurodegenerative disorders and may facilitate the development of therapeutic strategies targeting copper-mediated processes in protein aggregation and associated pathologies.

Crystal and Molecular Structures of Two Phthalocyanines, Chloro(phthalocyaninato)gallium(III) (ClGaPc) and µ-Oxobis(phthalocyaninato)gallium(III) (PcGaOGaPc)

The structure of µ-oxobis(phthalocyaninato)gallium(III) (PcGaOGaPc) and the structure of a second modification of chloro(phthalocyaninato)gallium(III) (ClGaPc) has been determined by single-crystal X-ray analysis. Sublimation of the respective compounds led to single crystals suitable for an X-ray study. Both compounds crystallize in the triclinic space group P1¯, with a unit cell for ClGaPc a = 13.770 Å, b = 13.770 Å, c = 14.039 Å, α = 98.32°, β = 108.64°, γ = 90.01°, containing four disordered molecules (Z = 4). The unit cell of the dimeric PcGaOGaPc contains one molecule, with half a molecule as an asymmetric moiety (Z = 2) and a = 7.848 Å, b = 12.529 Å, c = 12.720 Å, α = 91.03°, β = 94.94°, γ = 89.98°. The Ga atoms for the two ClGaPc molecules are placed 0.44 Å above the plane formed by the respective isoindole nitrogen N1 to N4. The two rings of the asymmetric unit (molecule 1 and 2) are arranged in parallel, with ca. 3.4 Å distance within the unit cell. The Ga-Cl bond distances are ca. 2.20 Å for the two molecules. The gallium of PcGaOGaPc is placed 0.49 Å above the respective isoindole nitrogen plane and the Ga-O bond amounts to 1.734 Å.