Volumetric Additive Manufacturing of Dicyclopentadiene by Solid-State Photopolymerization.

Polymerization in the solid state is generally infeasible due to restrictions on mobility. However, in this work, the solid-state photopolymerization of crystalline dicyclopentadiene is demonstrated via photoinitiated ring-opening metathesis polymerization. The source of mobility in the solid state is attributed to the plastic crystal nature of dicyclopentadiene, which yields local short-range mobility due to orientational degrees of freedom. Polymerization in the solid state enables photopatterning, volumetric additive manufacturing of free-standing structures, and fabrication with embedded components. Solid-state photopolymerization of dicyclopentadiene offers a new paradigm for advanced and freeform fabrication of high-performance thermosets.

Compact Solid Electrolyte Interface Realization Employing Surface-Modified Fillers for Long-Lasting, High-Performance All-Solid-State Li-Metal Batteries.

The implementation of polymer-based Li-metal batteries is hindered by their low coulombic efficiency and poor cycling stability attributed to continuous electrolyte decomposition. Enhancement of the solid electrolyte interface (SEI) stability is key to mitigating electrolyte decomposition. This study proposes surface-functionalized silica mesoball fillers to fabricate a composite polymer electrolyte (MSBM-CPE). As a result of surface modification, the polyethylene oxide matrix benefits from the uniform distribution of the filler, which provides a large surface area and Lewis acid sites. Molecular dynamics simulations reveal that the dissociation energy of lithium bis(trifluoromethanesulfonyl)imide in the filler is fourfold higher (-1.95 eV) than that of the filler-free electrolyte. Consequently, the MSMB-CPE diffusivity is 30 times higher than its filler-free counterpart. The MSMB-CPE of ionic conductivity of 1.16 × 10-2 S cm-1 @60 °C and a venerable Li-ion transference number of 0.81. The excellent compatibility of MSMB-CPE with the Li anode is demonstrated by its stable symmetric cell performance under high current density (200 µA cm-2 @60 °C) for over 5000 h. Approximately 85.60% retention capacity of the [Li/MSMB-CPE/LiFePO4] full cell after 700 cycles. Furthermore, compositional analysis reveals that the SEI layer in MSMB-CPE is smooth with fewer by-products at the electrolyte/Li interface.

Quasi-Solid-State Na-O2 Battery with Composite Polymer Electrolyte.

Na-O2 batteries have emerged as promising candidates due to their high theoretical energy density (1,601 Wh kg-1), the potential for high energy storage efficiency, and the abundance of sodium in the earth's crust. Considering the safety issue, quasi-solid-state composite polymer electrolytes are among the promising solid-state electrolyte candidates. Their higher mechanical toughness provides superior resistance to dendritic penetration compared with traditional liquid electrolytes. The flexibility of the composite polymer electrolyte matrix allows it to conform to various battery configurations and considerably reduces safety concerns related to the combustion risks associated with conventional liquid electrolytes. In this study, we employed poly(ethylene oxide) (PEO) and sodium bis(trifluoromethanesulfonyl)imide (NaTFSI) as the polymer matrix and sodium ion-conducting agent, respectively. We incorporated nanosized NZSP (25 wt %) to create the composite polymer electrolyte membrane. This CPE design facilitates ion conduction pathways through both sodium salt and NZSP. By utilizing a liquid electrolyte infiltration method, we successfully enhanced its ionic conductivity, achieving an ionic conductivity of 10-4 S cm-1 at room temperature.

Preparation and Evaluation of Berberine-Excipient Complexes in Enhancing the Dissolution Rate of Berberine Incorporated into Pellet Formulations.

Berberine is used in the treatment of metabolic syndrome and its low solubility and very poor oral bioavailability of berberine was one of the primary hurdles for its market approval. This study aimed to improve the solubility and bioavailability of berberine by preparing pellet formulations containing drug-excipient complex (obtained by solid dispersion). Berberine-excipient solid dispersion complexes were obtained with different ratios by the solvent evaporation method. The maximum saturation solubility test was performed as a key factor for choosing the optimal complex for the drug-excipient. The properties of these complexes were investigated by FTIR, DSC, XRD and dissolution tests. The obtained pellets were evaluated and compared in terms of pelletization efficiency, particle size, mechanical strength, sphericity and drug release profile in simulated media of gastric and intestine. Solid-state analysis showed complex formation between the drug and excipients used in solid dispersion. The optimal berberine-phospholipid complex showed a 2-fold increase and the optimal berberine-gelucire and berberine-citric acid complexes showed more than a 3-fold increase in the solubility of berberine compared to pure berberine powder. The evaluation of pellets from each of the optimal complexes showed that the rate and amount of drug released from all pellet formulations in the simulated gastric medium were significantly lower than in the intestine medium. The results of this study showed that the use of berberine-citric acid or berberine-gelucire complex could be considered a promising technique to increase the saturation solubility and improve the release characteristics of berberine from the pellet formulation.

Electrifying HCOOH synthesis from CO2 building blocks over Cu-Bi nanorod arrays.

Precise electrochemical synthesis of commodity chemicals and fuels from CO2 building blocks provides a promising route to close the anthropogenic carbon cycle, in which renewable but intermittent electricity could be stored within the greenhouse gas molecules. Here, we report state-of-the-art CO2-to-HCOOH valorization performance over a multiscale optimized Cu-Bi cathodic architecture, delivering a formate Faradaic efficiency exceeding 95% within an aqueous electrolyzer, a C-basis HCOOH purity above 99.8% within a solid-state electrolyzer operated at 100 mA cm-2 for 200 h and an energy efficiency of 39.2%, as well as a tunable aqueous HCOOH concentration ranging from 2.7 to 92.1 wt%. Via a combined two-dimensional reaction phase diagram and finite element analysis, we highlight the role of local geometries of Cu and Bi in branching the adsorption strength for key intermediates like *COOH and *OCHO for CO2 reduction, while the crystal orbital Hamiltonian population analysis rationalizes the vital contribution from moderate binding strength of η2(O,O)-OCHO on Cu-doped Bi surface in promoting HCOOH electrosynthesis. The findings of this study not only shed light on the tuning knobs for precise CO2 valorization, but also provide a different research paradigm for advancing the activity and selectivity optimization in a broad range of electrosynthetic systems.

Prediction of Novel Trigonal Chloride Superionic Conductors as Promising Solid Electrolytes for All-Solid-State Lithium Batteries.

Recently emerging lithium ternary chlorides have attracted increasing attention for solid-state electrolytes (SSEs) due to their favorable combination between ionic conductivity and electrochemical stability. However, a noticeable discrepancy in Li-ion conductivity persists between chloride SSEs and organic liquid electrolytes, underscoring the need for designing novel chloride SSEs with enhanced Li-ion conductivity. Herein, an intriguing trigonal structure (i.e., Li3SmCl6 with space group P3112) is identified using the global structure searching method in conjunction with first-principles calculations, and its potential for SSEs is systematically evaluated. Importantly, the structure of Li3SmCl6 exhibits a high ionic conductivity of 15.46 mS cm-1 at room temperature due to the 3D lithium percolation framework distinct from previous proposals, associated with the unique in-plane cation ordering and stacking sequences. Furthermore, it is unveiled that Li3SmCl6 possesses a wide electrochemical window of 0.73-4.30 V vs Li+/Li and excellent chemical interface stability with high-voltage cathodes. Several other Li3MCl6 (M = Er, and In) materials with isomorphic structures to Li3SmCl6 are also found to be potential chloride SSEs, suggesting the broader applicability of this structure. This work reveals a new class of ternary chloride SSEs and sheds light on strategy for structure searching in the design of high-performance SSEs.

Ni-Rich Layered Oxide Cathodes/Sulfide Electrolyte Interface in Solid-State Lithium Battery.

Because of the high specific capacity and low cost, Ni-rich layered oxide (NRLO) cathodes are one of the most promising cathode candidates for the next high-energy-density lithium-ion batteries. However, they face structure and interface instability challenges, especially the battery safety risk caused by using an intrinsic flammable organic liquid electrolyte. In this regard, a solid electrolyte with high safety is of great significance to promote the development of energy storage. Among them, sulfide electrolytes are considered to be the most potential substitutes for liquid electrolytes because of their high ionic conductivity and good processing properties. Nevertheless, the interfacial incompatibility between the sulfide electrolyte and NRLO cathode is the critical challenge for high-performance sulfide all-solid-state lithium batteries (ASSLBs). In this review, we summarize the problems of the Ni-rich cathode/sulfide solid electrolyte interface and the strategies to improve the interface stability. On the basis of these insights, we highlight the scientific problems and technological challenges that need to be resolved urgently and propose several potential directions to further improve the interface stability. The objective of this study is to provide a comprehensive understanding and insightful recommendations for the enhancement of the sulfide ASSLBs with NRLO cathode.

Selective correlations between aliphatic 13C nuclei in protein solid-state NMR.

Solid-state nuclear magnetic resonance (NMR) is a potent tool for studying the structures and dynamics of insoluble proteins. It starts with signal assignment through multi-dimensional correlation experiments, where the aliphatic 13Cα-13Cß correlation is indispensable for identifying specific residues. However, developing efficient methods for achieving this correlation is a challenge in solid-state NMR. We present a simple band-selective zero-quantum (ZQ) recoupling method, named POST-C4161 (PC4), which enhances 13Cα-13Cß correlations under moderate magic-angle spinning (MAS) conditions. PC4 requires minimal 13C radio-frequency (RF) field and proton decoupling, exhibits high stability against RF variations, and achieves superior efficiency. Comparative tests on various samples, including the formyl-Met-Leu-Phe (fMLF) tripeptide, microcrystalline ß1 immunoglobulin binding domain of protein G (GB1), and membrane protein of mechanosensitive channel of large conductance from Methanosarcina acetivorans (MaMscL), demonstrate that PC4 selectively enhances 13Cα-13Cß correlations by up to 50 % while suppressing unwanted correlations, as compared to the popular dipolar-assisted rotational resonance (DARR). It has addressed the long-standing need for selective 13C-13C correlation methods. We anticipate that this simple but efficient PC4 method will have immediate applications in structural biology by solid-state NMR.

Inhibition mechanism of different structural polyphenols against α-amylase studied by solid-state NMR and molecular docking.

Polyphenol has the considerable effects for inhibition of digestive enzymes, however, inhibition mechanism of molecular size-dependent polyphenols on enzyme activity is still lacking. Herein, inhibition effect and binding interactions of three different structural polyphenols (catechol, quercetin and hesperidin) on α-amylase were studied. Inhibition assays proved that polyphenols significantly inhibited α-amylase and their effects were increased with their molecular sizes. Hesperidin showed the highest inhibition ability of α-amylase, which was determined as IC50 = 0.43 mg/mL. Fluorescence and FT-IR spectroscopy proved that inter-molecular interactions between polyphenols and α-amylase occurred through non-covalent bonds. Besides, the secondary structure of α-amylase was obviously changed after binding with polyphenols. Inter-molecular interactions were investigated using solid-state NMR and molecular docking. Findings proved that hydrogen bonds and π-π stacking interactions were the mainly inter-molecular interactions. We hope this contribution could provide a theoretical basis for developing some digestive enzyme inhibitors from natural polyphenols.

Cross polarization stability in multidimensional NMR spectroscopy of biological solids.

Magic-angle spinning (MAS) solid-state nuclear magnetic resonance (SSNMR) spectroscopy is a powerful and versatile technique for probing structure and dynamics in large, insoluble biological systems at atomic resolution. With many recent advances in instrumentation and polarization methods, technology development in SSNMR remains an active area of research and presents opportunities to further improve data collection, processing, and analysis of samples with low sensitivity and complex tertiary and quaternary structures. SSNMR spectra are often collected as multidimensional data, requiring stable experimental conditions to minimize signal fluctuations (t1 noise). In this work, we examine the factors adversely affecting signal stability as well as strategies used to mitigate them, considering laboratory environmental requirements, configuration of amplifiers, and pulse sequence parameter selection. We show that Thermopad® temperature variable attenuators (TVAs) can partially compensate for the changes in amplifier output power as a function of temperature and thereby ameliorate one significant source of instability for some spectrometers and pulse sequences. We also consider the selection of tangent ramped cross polarization (CP) waveform shapes, to balance the requirements of sensitivity and instrumental stability. These findings collectively enable improved stability and overall performance for CP-based multidimensional spectra of microcrystalline, membrane, and fibrous proteins performed at multiple magnetic field strengths.

Low power supercycled TPPM decoupling.

Improving the spectral sensitivity and resolution of biological solids is one of the long-standing problems in nuclear magnetic resonance (NMR) spectroscopy. In this report, we introduce low-power supercycled variants of two-pulse phase-modulated (TPPM) sequence for heteronuclear decoupling. The utility of the sequence is shown by improvements in the transverse relaxation time of observed nuclei (with 1H decoupling) with its application to different samples (uniformly 13C, 15N, 2H-labeled GB1 back-exchanged with 25% H2O and 75% D2O, uniformly 13C, 15N, 2H-labeled human derived Asyn fibril back-exchanged with 100% H2O and uniformly 13C, 15N -labeled human derived Asyn fibril) at fast MAS using low radiofrequency (RF) fields. To understand the effect of spinning speed, the transverse relaxation time is monitored under different spinning frequencies. In comparison to existing heteronuclear decoupling sequences, the supercycled TPPM (sTPPM) sequence significantly improves the spectral sensitivity and resolution and is robust towards B1 inhomogeneity and decoupler offset.

Optimization of Porous Structures of Carbon Matrices for Loading Red Phosphorus to Achieve High-Capacity and Long-Life Anodes for All-Solid-State Lithium-Ion Batteries.

All-solid-state lithium-ion batteries (ASSLIBs) using sulfide electrolytes and high-capacity alloy-type anodes have attracted sizable interest due to their potential excellent safety and high energy density. Encapsulating insulating red phosphorus (P) inside nanopores of a carbon matrix can adequately activate its electrochemical alloying reaction with lithium. Therefore, the porosity of the carbon matrix plays a crucial role in the electrochemical performance of the resulting red P/carbon composites. Here, we use zeolite-templated carbon (ZTC) with monodisperse micropores and mesoporous carbon (CMK-3) with uniform mesopores as the model hosts of red P. Our results reveal that micropores enable more effective pore utilization for the red P loading, and the P@ZTC material can achieve a record-high content (65.0 wt %) of red P confined within pores. When used as an anode of ASSLIBs, the P@ZTC electrode delivers an ultrahigh capacity of 1823 mA h g-1 and a high initial Coulombic efficiency of 87.44%. After 400 deep discharge-charge cycles (running over 250 days) at 0.2 A g-1, the P@ZTC electrode still holds a reversible capacity of 1260 mA h g-1 (99.92% capacity retention per cycle). Moreover, a P@ZTC||LiNi0.8Co0.1Mn0.1O2 full cell can deliver a reversible areal capacity of over 3 mA h cm-2 at 0.1C after 100 cycles.

Response surface methodology and machine learning optimisations comparisons of recycled AA6061-B4C-ZrO2 hybrid metal matrix composites via hot forging forming process.

The optimal conditions of applied factors to reuse Aluminium AA6061 scraps are (450, 500, and 550) °C preheating temperature, (1-15) % Boron Carbide (B4C), and Zirconium (ZrO2) hybrid reinforced particles at 120 min forging time via Hot Forging (HF) process. The response surface methodology (RSM) and machine learning (ML) were established for the optimisations and comparisons towards materials strength structure. The Ultimate Tensile Strength (UTS) strength and Microhardness (MH) were significantly increased by increasing the processed temperature and reinforced particles because of the material dispersion strengthening. The high melting point of particles caused impedance movements of aluminium ceramics dislocations which need higher plastic deformation force and hence increased the material's mechanical and physical properties. But, beyond Al/10 % B4C + 10 % ZrO2 the strength and hardness were decreased due to more particle agglomeration distribution. The optimisation tools of both RSM and ML show high agreement between the reported results of applied parameters towards the materials' strength characterisation. The microstructure analysis of Field Emission Scanning Electron Microscopy (FE-SEM) and Atomic Force Microscope (AFM) provides insights mapping behavioural characterisation supports related to strength and hardness properties. The distribution of different volumes of ceramic particle proportion was highlighted. The environmental impacts were also analysed by employing a life cycle assessment (LCA) to identify energy savings because of its fewer processing steps and produce excellent hybrid materials properties.

Pathological mutations in the phospholamban cytoplasmic region affect its topology and dynamics modulating the extent of SERCA inhibition.

Phospholamban (PLN) is a 52 amino acid regulin that allosterically modulates the activity of the sarco(endo)plasmic reticulum Ca2+-ATPase (SERCA) in the heart muscle. In its unphosphorylated form, PLN binds SERCA within its transmembrane (TM) domains, approximately 20 Šaway from the Ca2+ binding site, reducing SERCA's apparent Ca2+ affinity (pKCa) and decreasing cardiac contractility. During the enzymatic cycle, the inhibitory TM domain of PLN remains anchored to SERCA, whereas its cytoplasmic region transiently binds the ATPase's headpiece. Phosphorylation of PLN at Ser16 by protein kinase A increases the affinity of its cytoplasmic domain to SERCA, weakening the TM interactions with the ATPase, reversing its inhibitory function, and augmenting muscle contractility. How the structural changes caused by pathological mutations in the PLN cytoplasmic region are transmitted to its inhibitory TM domain is still unclear. Using solid-state NMR spectroscopy and activity assays, we analyzed structural and functional effects of a series of mutations and their phosphorylated forms located in the PLN cytoplasmic region and linked to dilated cardiomyopathy. We found that these missense mutations affect the overall topology and dynamics of PLN and ultimately modulate its inhibitory potency. Also, the changes in the TM tilt angle and cytoplasmic dynamics of PLN caused by these mutations correlate well with the extent of SERCA inhibition. Our study unveils new molecular determinants for designing variants of PLN that outcompete endogenous PLN to regulate SERCA in a tunable manner.

Exploring the influence of hydrogen bond donor groups on the microstructure and intermolecular interactions of amorphous solid dispersions containing diflunisal structural analogues.

Drug-polymer intermolecular interactions, and H-bonds specifically, play an important role in the stabilization process of a compound in an amorphous solid dispersion (ASD). However, it is still difficult to predict whether or not interactions will form and what the strength of those interactions would be, based on the structure of drug and polymer. Therefore, in this study, structural analogues of diflunisal (DIF) were synthesized and incorporated in ASDs with poly(vinylpyrrolidone-co-vinyl acetate) (PVPVA) as a stabilizing polymer. The respective DIF derivatives contained different types and numbers of H-bond donor groups, which allowed to assess the influence of these structural differences on the phase behavior and the actual interactions formed in the ASDs. The highest possible drug loading of these derivatives in PVPVA were evaluated through film casting. Subsequently, a lower drug loading of each compound was spray dried. These spray dried ASDs were subjected to an in-depth solid-state nuclear magnetic resonance (ssNMR) study, including 1D spectroscopy and relaxometry, as well as 2D dipolar HETCOR experiments. The drug loading study revealed the highest possible loading of 50 wt% for the native DIF in PVPVA. The methoxy DIF derivative reached the second highest drug loading of 35 wt%, while methylation of the carboxyl group of DIF led to a sharp decrease in the maximum loading, to around 10 wt% only. Unexpectedly, the maximum loading increased again when both the COOH and OH groups of diflunisal were methylated in the dimethyl DIF derivative, to around 30 wt%. The ssNMR study on the spray dried ASD samples confirmed intermolecular H-bonding with PVPVA for native DIF and methoxy DIF. Studies of the proton relaxation decay times and 2D 1H-13C dipolar HETCOR experiments indicated that the ASDs with native DIF and methoxy DIF were homogenously mixed, while the ASDs containing DIF methyl ester and dimethyl DIF were phase separated at the nm level. It was established that, for these systems, the availability of the carboxyl group was imperative in the formation of intermolecular H-bonds with PVPVA and in the generation of homogenously mixed ASDs.

Large Molecular Rotation in Crystal Changes the Course of a Topochemical Diels-Alder Reaction from a Predicted Polymerization to an Unexpected Intramolecular Cyclization.

A designed anthracene-based monomer for topochemical Diels-Alder cycloaddition polymerization crystallized with head-to-tail arrangement of molecules, as revealed by single-crystal X-ray diffraction (SCXRD) analysis. The diene and dienophile units of adjacent monomer molecules are aligned at an average distance of 4.6 Å, suggesting a favorable crystalline arrangement for their intermolecular Diels-Alder cycloaddition reaction to form a linear polymer . Surprisingly, heating the monomer crystals at a temperature above 125 °C resulted in the formation of intramolecular Diels-Alder cycloadduct, which could be characterized by various spectroscopy and SCXRD analysis. Various time-dependent studies such as NMR, PXRD, and DSC, studies established that the reaction followed topochemical pathway. Schmidt's topochemical postulates are generally used to predict the topochemical reactivity and product, by analyzing the crystal structure of the reactant. Though the crystal arrangement predicted polymerization, upon heating the molecule avoided this pathway by undergoing a large rotation to form an intramolecular cycloadduct. Theoretical calculations supported the feasibility of the rotation, exploiting the flexibility of the molecule and voids present. These findings caution that the reliance on Schmidt's criteria for topochemical reactions may sometimes be misleading, especially in heat-induced reactions.

Building Solid-State Batteries: Insights from Swiss Research Labs.

This review article delves into the growing field of solid-state batteries as a compelling alternative to conventional lithium-ion batteries. The article surveys ongoing research efforts at renowned Swiss institutions such as ETH Zurich, Empa, Paul Scherrer Institute, and Berner Fachhochschule covering various aspects, from a fundamental understanding of battery interfaces to practical issues of solid-state battery fabrication, their design, and production. The article then outlines the prospects of solid-state batteries, emphasizing the imperative practical challenges that remain to be overcome and highlighting Swiss research groups' efforts and research directions in this field.

Solvent-Mediated Synthesis and Characterization of Li3InCl6 Electrolytes for All-Solid-State Li-Ion Battery Applications.

Superionic halides have attracted widespread attention as solid electrolytes due to their excellent ionic conductivity, soft texture, and stability toward high-voltage electrode materials. Among them, Li3InCl6 has aroused interest since it can be easily synthesized in water or ethanol. However, investigations into the influence of solvents on both the crystal structure and properties remain unexplored. In this work, Li3InCl6 is synthesized by three different solvents: water, ethanol, and water-ethanol mixture, and the difference in properties has been studied. The results show that the product obtained by the ethanol solvent demonstrates the largest unit cell parameters with more vacancies, which tend to crystallize on the (131) plane and provide the 3D isotropic network migration for lithium-ions. Thus, it exhibits the highest ionic conductivity (1.06 mS cm-1) at room temperature and the lowest binding energy (0.272 eV). The assembled all-solid-state lithium metal batteries (ASSLMBs) employing Li3InCl6 electrolytes demonstrate a high initial discharge capacity of 153.9 mA h g-1 at 0.1 C (1 C = 170 mA h g-1) and the reversible capacity retention rate can reach 82.83% after 50 cycles. This work studies the difference in ionic conductivity between Li3InCl6 electrolytes synthesized by different solvents, which can provide a reference for the future synthesis of halide electrolytes and enable their practical application in halide-based ASSLMBs with a high energy density.

Synthesis of Intrinsically-Fluorescent Aliphatic Tautomeric Polymers for Proton-Conductivity, Dual-State Emission, and Sensing/Oxidation-Reduction of Metal Ions.

Herein, fluorescent conducting tautomeric polymers (FCTPs) are developed by polymerizing 2-methylprop-2-enoic acid (MPEA), methyl-2-methylpropenoate (MMP), N-(propan-2-yl)prop-2-enamide (PPE), and in situ-anchored 3-(N-(propan-2-yl)prop-2-enamido)-2-methylpropanoic acid (PPEMPA). Among as-synthesized FCTPs, the most promising characteristics in FCTP3 are confirmed by NMR and Fourier transform infrared (FTIR) spectroscopies, luminescence enhancements, and computational studies. In FCTP3, ─C(═O)NH─, -C(═O)N<, ─C(═O)OH, and ─C(═O)OCH3 subluminophores are identified by theoretical calculations and experimental analyses. These subluminophores facilitate redox characteristics, solid state emissions, aggregation-enhanced emissions (AEEs), excited-state intramolecular proton transfer (ESIPT), and conductivities in FCTP3. The ESIPT-associated dual emission/AEEs of FCTP3 are elucidated by time correlated single photon counting (TCSPC) investigation, solvent polarity effects, concentration-dependent emissions, dynamic light scattering (DLS) measurements, field emission scanning electron microscopy images, and computational calculations. The cyclic voltammetry measurements of FCTP3 indicate cumulative redox efficacy of ─C(═O)OH, ─C(═O)NH─/-C(═O)N<, ─C(─O─)═NH+─/─C(─O─)═N+, and ─C(═N)OH functionalities. In FCTP3, ESIPT-associated dual-emission enable in the selective detection of Cr(III)/Cu(II) at λem1/λem2 with the limit of detection of 0.0343/0.079 ppb. The preferential interaction of Cr(III)/Cu(II) with FCTP3 (amide)/FCTP3 (imidol) and oxidation/reduction of Cr(III)/Cu(II) to Cr(VI)/Cu(I) are further supported by NMR-titration; FTIR and X-ray photoelectron spectroscopy analyses; TCSPC/electrochemical/DLS measurement; alongside theoretical calculations. The proton conductivity of FCTP3 is explored by electrochemical impedance spectroscopy and I-V measurements.

Solid-state NMR backbone chemical shift assignments of α-synuclein amyloid fibrils at fast MAS regime.

The α-synuclein (α-syn) amyloid fibrils are involved in various neurogenerative diseases. Solid-state NMR (ssNMR) has been showed as a powerful tool to study α-syn aggregates. Here, we report the 1H, 13C and 15N back-bone chemical shifts of a new α-syn polymorph obtained using proton-detected ssNMR spectroscopy under fast (95 kHz) magic-angle spinning conditions. The manual chemical shift assignments were cross-validated using FLYA algorithm. The secondary structural elements of α-syn fibrils were calculated using 13C chemical shift differences and TALOS software.