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Moreover, trinuclear 2- or 4-methylimidazole oxothiomolybdenum(IV) glycolates 1 and 3 show only a few adsorptions for O2 under the same conditions.The designed synthesis of nanotwin architectures and thus-induced phase junctions expresses huge significance for semiconductor photocatalysts. However, current methods of producing nanotwins mainly involve high-temperature thermal treatment and tedious reaction steps, generally resulting in large bulk structure with ill-defined morphology and low specific surface area. Here, we propose a mild ligand-assisted coordinative self-assembly method to synthesize uniform mesoporous ZnxCd1-xS nanospheres with ultrahigh surface areas (148-312 m2 g-1) and controllable diameter (90-370 nm). Moreover, the sample possesses abundant phase junctions induced by nanotwins containing both hexagonal and cubic segments. With the synergy of the twin-induced phase junctions and high surface area, the as-prepared mesoporous Zn0.82Cd0.18S nanospheres exhibit a remarkable photocatalytic H2 evolution rate of 13.46 mmol h-1 g-1 with free noble metal. The mechanism of photocarrier dynamics was studied by transient photovoltage spectroscopy, manifesting that the photocarrier lifetime of Zn0.82Cd0.18S is largely prolonged and therefore improves the charge separation efficiency and photocatalytic activity.Fluorocarbons and chlorocarbons are common volatile organic compounds that pose serious risk to the environment and human health and therefore need to be effectively captured. Herein, we report a series of highly fluorinated metal-organic frameworks with high porosity (Brunauer-Emmett-Teller surface area ∼3000 m2/g) and stability. They show exceptionally high capacity and good recyclability toward the adsorption of fluorocarbons and chlorocarbons.In our efforts to understand the nature of metal thiolates, we have explored the chemistry of cobalt ion supported by (thiolato)phosphine ligand derivatives. Herein, we synthesized and characterized a square-planar CoII complex binding with a bidentate (thiolato)phosphine ligand, Co(PS1″)2 (1) ([PS1″]- = [P(Ph)2(C6H3-3-SiMe3-2-S)]-). The complex activates O2 to form a ligand-based oxygenation product, Co(OPS1″)2 (2) ([OPS1″]- = [PO(Ph)2(C6H3-3-SiMe3-2-S)]-). In addition, an octahedral CoIII complex with a tridentate bis(thiolato)phosphine ligand, [NEt4][Co(PS2*)2] (3) ([PS2*]2- = [P(Ph)(C6H3-3-Ph-2-S)2]2-), was obtained. Compound 3 cleaves the C-Cl bond in dichloromethane via an S-based nucleophilic attack to generate a chloromethyl thioether group. Two isomeric products, [Co(PS2*)(PSSCH2Cl*)] (4 and 4') ([PSSCH2Cl*]- = [P(Ph)(C6H3-3-Ph-2-S)(C6H3-3-Ph-2-SCH2Cl)]-), were isolated and fully characterized. Both transformations, oxygenation of a CoII-bound phosphine donor in 1 and alkylation of a CoIII-bound thiolate in 3, were monitored by spectroscopic methods. These reaction products were isolated and fully characterized. Density functional theory (DFT, the B3LYP functional) calculations were performed to understand the electronic structure of 1 as well as the pathway of its transformation to 2.The reaction of PMe3 or PPh3 with PF5 in anhydrous CH2Cl2 or hexane forms the white, moisture-sensitive complexes [PF5(PR3)] (R = Me, Ph). Similar reactions involving the diphosphines o-C6H4(PR2)2 afford the complexes [PF4o-C6H4(PR2)2][PF6]. The X-ray structures of [PF5(PR3)] and [PF4o-C6H4(PMe2)2][PF6] show pseudo-octahedral fluorophosphorus centers. Multinuclear NMR spectra (1H, 19F1H, 31P1H) show that in solution in CH2Cl2/CD2Cl2 the structures determined crystallographically are the only species present for [PF5(PMe3)] and [PF4o-C6H4(PMe2)2][PF6] but that [PF5(PPh3)] and [PF4o-C6H4(PPh2)2][PF6] exhibit reversible dissociation of the phosphine at ambient temperatures, although exchange slows at low temperatures. HDAC inhibitor The complex 19F1H and 31P1H NMR spectra have been analyzed, including those of the cation [PF4o-C6H4(PMe2)2]+, which is a second-order AA'XX'B2M spin system. The unstable [PF5(AsMe3)], which decomposes in a few hours at ambient temperatures, has also been isolated and spectroscopically characterized; neither AsPh3 nor SbEt3 forms similar complexes. The electronic structures of the PF5 complexes have been explored by DFT calculations. The DFT optimized geometries for [PF5(PMe3)], [PF5(PPh3)], and [PF4o-C6H4(PMe2)2]+ are in good agreement with their respective crystal structure geometries. DFT calculations on the PF5-L complexes reveal the P-L bond strength falls with L in the order PMe3 > PPh3 > AsMe3, consistent with the experimentally observed stabilities, and in the PF5-L complexes, electron transfer from L to PF5 on forming these complexes also follows the order PMe3 > PPh3 ≈ AsMe3.ε-Fe2O3, a metastable phase of iron oxide, is widely known as a room-temperature multiferroic material or as a superhard magnet. Element substitution into ε-Fe2O3 has been reported in the literature; however, the substituted ions have a strong site preference depending on their ionic radii and valence. In this study, in order to characterize the crystal structure and magnetic properties of ε-Fe2O3 in the Fe2+/Fe3+ coexisting states, Li+ was electrochemically inserted into ε-Fe2O3 to reduce Fe3+. The discharge and charge of Li+ into/from ε-Fe2O3 revealed that Li+ insertion was successful. X-ray magnetic circular dichroism results indicated that the reduced Fe did not exhibit site preference. Increasing the Li+ content in ε-Fe2O3 resulted in decreased saturation magnetization and irregular variation of the coercive field. We present a comprehensive discussion of how magnetic properties are modified with increasing Li+ content using transmission electron microscopy images and considering the Li+ diffusion coefficient. The results suggest that inserting Li+ into crystalline ε-Fe2O3 is a useful tool for characterizing crystal structure, lithiation limit, and magnetic properties in the coexistence of Fe2+/Fe3+.Several new materials with four structure-types (e.g., Cu0.32In1.74Ga0.84S4 (CIGS4), Cu0.65In1.75Ga1.4S5 (CIGS5), Cu1.44In2.77Ga0.76S6 (CIGS6), and Cu1.1In2.49Ga1.8S7 (CIGS7)) have been evidenced in the Cu2S-In2S3-Ga2S3 pseudo-ternary system. All of them present a 2D structure built upon infinite 2/∞[InS2] layers ((InS6) octahedra sharing edges) on which condense on both sides mono-, bi-, or tri-2/∞[MS] layers ((MS4) tetrahedra (M = Cu, In, Ga) sharing corners). (M(Td))n-2(In(Oh))Sn slabs are separated from each other by a van der Waals gap, and subscript n refers to the number of sulfur layers within the building block. These compounds have the propensity to display stacking faults but also polymorphic forms. Their optical gap (ca. 1.7 eV) is quite similar to the one of the Cu(In0.7Ga0.3)S2 chalcopyrite absorbers used in tandem solar cells, and the major charge carriers are holes. This suggests that they might be very attractive for photovoltaic applications in thin film devices but also for photocatalysis.Using density functional theory calculations, we propose that the exposed Ga atom in a two-dimensional defective gallium selenide monolayer (V-GaSe) can display a good dinitrogen fixation capacity and an excellent nitrogen reduction reaction (NRR) performance. Our results show that N2 can be captured by three sp3-hybridized Ga atoms due to the pulling effect. With the enlargement in vacancy size through applying tensile strain, the adsorption of N2 is strengthened and the electrochemical NRR performance is enhanced. On 8% strained V-GaSe, the estimated onset potential is as low as 0.30 V. Inspired by the concept of "defect-size-dependent" NRR performance, we further design a Janus V-GaInSe2 structure in which the natural size of the cavity is enlarged and the electron density of the active Ga atoms is enriched. It is found that N2 adsorption is demonstrably enhanced with respect to V-GaSe. On 4% strained V-GaInSe2, the onset potential is calculated to be 0.31 V, which is the same as the 8% strained V-GaSe. Moreover, the produced NH3 can be removed rapidly with a free-energy change of less than 0.52 eV, which is much lower than those of most reported catalysts with low overpotentials. Meanwhile, the side hydrogen evolution reaction is successively suppressed as the strain increases. Our work offers a feasible method that utilizes the size of a defect to tune the NRR performance, adding a new understanding of N2 fixation and sustainable NH3 production.A catalyst-free organosolv pulping process was applied to cup plant (Silphium perfoliatum, S), Miscanthus grass (Miscanthus x giganteus, M), and the Paulownia tree (Paulownia tomentosa, P), resulting in high-purity lignins with no signals for cellulose, hemicellulose, or other impurities in two-dimensional heteronuclear single quantum coherence (HSQC) nuclear magnetic resonance (NMR) spectra. Different biomass particle sizes used for the organosolv pulping (1.6-2.0 mm (1); 0.5-1.0 mm (2); less then 0.25 mm (3)) influenced the molecular weight and chemical structure of the isolated lignins. Principal component analysis (PCA) of 1H NMR data revealed a high intergroup variance of Miscanthus and Paulownia lignins, separating the small particle fraction from the larger ones. Furthermore, monolignol ratios identified via HSQC NMR differ significantly Miscanthus lignins were composed of all three monolignols (guaiacyl (G), p-hydroxyphenyl (H), syringyl (S)), while for Paulownia and Silphium lignins only G and S units were observed (except for P3).Apohemoglobin (apoHb) contains vacant hydrophobic heme-binding pockets that can bind to a variety of hydrophobic molecules. Thus, apoHb is a promising protein for drug delivery, bioimaging, and heme scavenging. Unfortunately, apoHb has a short half-life and precipitates at physiological temperature. In this study, apoHb was surface-conjugated with poly(ethylene glycol) (PEG) to improve the therapeutic potential of apoHb. The scalable PEGylation process had >95% protein yield with ∼10 to 12 PEGs attached to each apoHb αβ dimer. The resulting PEG-apoHb had an average molecular weight of ∼80 to 90 kDa and a hydrodynamic diameter of 11 nm. PEG-apoHb maintained high heme-binding affinity and 30-40% of the heme-binding activity. Moreover, heme-bound and heme-free PEG-apoHb bound to haptoglobin, enabling PEG-apoHb to potentially target CD163+ macrophages and monocytes. Finally, PEG-apoHb was stable at physiological temperature with minimal precipitation. In summary, the in vitro results shown demonstrate that PEG-apoHb could be an effective in vivo heme scavenger during states of hemolysis.Femtosecond-laser ionization mass spectrometry (fs-LIMS) is demonstrated to be a powerful analytical method providing access to the qualitative distinction of structural isomers of ortho-, meta-, and para-fluorotoluene. The key point of the approach presented is a systematic variation of the spectral phase of the fs-laser pulses, which characteristically affects the fragmentation pattern observed in the mass spectra. Variation of the linear chirp parameter is also helpful for rationalizing the fragmentation mechanism. Ultimately two ternary mixtures of the three title isomers are quantitatively analyzed in situ with an accuracy of 5% for the molar fractions.
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