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Discussing the fundamental and practical differences, we demonstrate the degree of complementarity of the techniques.Upon reaction with copper(i), peri-halo naphthyl phosphines readily form peri-bridged naphthyl phosphonium salts. The reaction works with alkyl, aryl and amino substituents at phosphorus, with iodine, bromine and chlorine as a halogen. It proceeds under mild conditions and is quantitative, despite the strain associated with the resulting 4-membered ring structure and the naphthalene framework. The transformation is amenable to catalysis. Under optimized conditions, the peri-iodo naphthyl phosphine 1-I is converted into the corresponding peri-bridged naphthyl phosphonium salt 2b in only 5 minutes at room temperature using 1 mol% of CuI. Based on DFT calculations, the reaction is proposed to involve a Cu(i)/Cu(iii) cycle made of P-coordination, C-X oxidative addition and P-C reductive elimination. This copper-catalyzed route gives a general and efficient access to peri-bridged naphthyl phosphonium salts for the first time. Reactivity studies could thus be initiated and the possibility to insert gold into the strained P-C bond was demonstrated. It leads to (P,C)-cyclometallated gold(iii) complexes. According to experimental observations and DFT calculations, two mechanistic pathways are operating (i) direct oxidative addition of the strained P-C bond to gold,(ii) backward-formation of the peri-halo naphthyl phosphine (by C-P oxidative addition to copper followed by C-X reductive elimination), copper to gold exchange and oxidative addition of the C-X bond to gold. Detailed analysis of the reaction profiles computed theoretically gives more insight into the influence of the nature of the solvent and halogen atom, and provides rationale for the very different behaviour of copper and gold in this chemistry.Correction for 'Metallosupramolecules of pillar[5]-bis-trithiacrown including a mercury(ii) iodide ion-triplet complex' by Mingyeong Shin et al., Chem. Commun., 2020, DOI 10.1039/d0cc03902k.The consecutive activation of B-H bonds in mesitylborane (H2BMes; Mes = 2,4,6-(CH3)3C6H2) by a 16-electron rhodium(i) monocarbonyl complex, (iPrNNN)Rh(CO) (1-CO; iPrNNN = 2,5-[iPr2P[double bond, length as m-dash]N(4-iPrC6H4)]2N(C4H2)-) is described. Dehydrogenative extrusion of the BMes fragment led to the isolation of (iPrNNN)(CO)RhBMes (1-BMes). https://www.selleckchem.com/products/gne-049.html Addition of H2 gas to 1-BMes regenerated 1-CO and H2BMes, highlighting the ability of 1-CO to facilitate interconversion of BMes with dihydrogen. Reactivity studies revealed that 1-BMes promotes formal group transfer and that BAr fragments accessed by dehydrogenation are reactive entities.The surface characteristics of electrodes vary depending on the solvent used. Furthermore, electrochemical performance varies depending on the surface morphology of the electrode. In this study, we grew 3D binary NiCu-based composites on Ni foam, via a binder-free hydrothermal method, for use as a cathode in high-performance supercapacitors. We employed different solvents to prepare the electrodes by adjusting the ratio of deionized water (DI water) to methanol. The electrode prepared using DI water as the solvent had the largest surface area with a nanowire structure. This morphology allowed for good electrical performance by greatly improving the electrode and electrolyte contact area and shortening the ion diffusion path. The optimized deposition of NiCu(CO3)(OH)2 nanowires (50 mL of DI water as solvent) showed an excellent maximum specific capacity of 758.9 mA h g-1 at a current density of 3 A g-1, as well as outstanding cycling performance with 87.2% retention after 5000 cycles. In this work, we focused on the large specific surface area and suitable electrochemical properties of NiCu(CO3)(OH)2 electrodes with various solvents. As a result, the asymmetric supercapacitor (ASC) using the NiCu(CO3)(OH)2 electrode prepared with 50 ml of DI water as the solvent as the positive electrode and graphene as the negative electrode, exhibited an energy density of 26.7 W h kg-1 at a power density of 2534 W kg-1, and excellent cycling stability with 91.3% retention after 5000 cycles. The NiCu(CO3)(OH)2//graphene ASC could turn on an LED light and demonstrated better electrical performance than most previously reported nickel- and copper-based carbonate hydroxide ASCs. In addition, in the present scenario where many nanoscale studies are conducted, a method of controlling the nanostructure of a material through facile solvent control will be of great help to many researchers.Once a suitable experimental design has been used to find the most important factors affecting the outcome of an experiment, and maybe to find any significant interactions between them, we can use an optimisation method to find the best levels (values) for those factors. This Technical Brief outlines the basic principles of optimisation, and introduces some of the most commonly used approaches.This paper proposes for the first time (a) a qualitative analytical method based on portable and benchtop backscattering Raman spectrometers coupled to hierarchical cluster analysis (HCA) and multivariate curve resolution - alternating least-squares (MCR-ALS) to identify two polymorphs of antimalarial quinine sulfate in commercial pharmaceutical tablets in their intact forms and (b) a quantitative analytical method based on gold nanoparticles (AuNPs) as active substrates for surface-enhanced Raman scattering (SERS) in combination with MCR-ALS to quantify quinine sulfate in commercial pharmaceutical tablets in solution. The pure concentration and spectral profiles recovered by MCR-ALS proved that both formulations present different polymorphs. These results were also confirmed by two clusters observed in the HCA model, according to their similarities within and among the samples that provided useful information about the homogeneity of different pharmaceutical manufacturing processes. AuNPs-SERS coupled to MCR-ALS was able to quantify quinine sulfate in the calibration range from 150.00 to 200.00 ng mL-1 even with the strong overlapping spectral profile of the background SERS signal, proving that it is a powerful ultrahigh sensitivity analytical method. This reduced linearity was validated throughout a large calibration range from 25.00 to 175.00 μg mL-1 used in a reference analytical method based on high performance liquid chromatography with a diode array detector (HPLC-DAD) coupled to MCR-ALS for analytical validation purposes, even in the presence of a coeluted compound. The analytical methods developed herein are fast, because second-order chromatographic data and first-order SERS spectroscopic data were obtained in less than 6 and 2 min, respectively. Concentrations of quinine sulfate were estimated with low root mean square error of prediction (RMSEP) values and a low relative error of prediction (REP%) in the range 1.8-4.5%.
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