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1.
After more than 50 years, the synthesis and electronic structure of the first and only reported “U0 complex” [U(bipy)4] ( 1 ) has been reinvestigated. Additionally, its one‐electron reduced product [Na(THF)6][U(bipy)4] ( 2 ) has been newly discovered. High resolution crystallographic analyses combined with magnetic and computational data show that 1 and its derivative 2 are best described as highly reduced species containing mid‐to‐high‐valent uranium ligated by redox non‐innocent ligands.  相似文献   
2.
Understanding the interaction between chitosan molecules and sodium silicate is one of the principal objectives for the development of new environmentally benign strategies for the synthesis of low-cost porous silica with hierarchical structure. In this work, we have explored two essential factors simultaneously: chitosan/silica ratios (0.1, 0.4, 0.8 and 1.6) and pH values of the mixture (3, 5 and 6). The obtained silica–chitosan composite and the calcined products were investigated by using thermal gravimetric analysis, N2-physisorption, scanning electron microscopy, and transmission electron microscopy. Rapid precipitation of silica–chitosan composite occurred because of the initial pH values of the chitosan and sodium silicate solutions. The amount of precipitating silica–chitosan composite was increased with increasing pH value of the mixture and chitosan/silica ratios but it did not change with the decrease of pH value of the mixture. The as-synthesized products prepared at pH 3 and 6 showed macroscopic two-solid phases (consisting of silica-rich phase and chitosan-rich phase), while those prepared at pH 5 displayed liquid and solid phases. At pH 3, a unimodal porous structure was found for the calcined products obtained from the silica-rich phase while a hierarchical structure was found for those obtained from the chitosan-rich phase; meanwhile, a hierarchical structure occurred for all calcined products prepared at pH 6. Different hierarchical structures of the silica products could be obtained by changing pH value of the mixture and chitosan/silica ratios.  相似文献   
3.
4.
In this study, the formation of silica–chitosan hybrid materials via sol–gel process under pH values of 2–6 were investigated using N2 sorption analysis, scanning electron microscopy, transmission electron microscopy, thermal analysis and zeta potential analyzer. The hierarchical structure consisting of meso- and macropore was formed when pH value was higher than 2. Mesopores were formed as the interparticle channels of silica nanoparticles aggregates, whereas macropores were the void between the aggregates (clusters). The clusters size was decreased with increasing the pH value, resulting in the increase of the macroporosity. The thermal conductivity of the products was controlled in the range of 0.06 and 0.13 W m−1 K−1 by varying the product porosity between 88 and 69% (pH 6 and pH 2, respectively).  相似文献   
5.
Two‐electron reduction of the TiIV compound (ketguan)(ImDippN)Ti(OTf)2 ( 3 ) gives the arene‐masked complex (ketguan)(η6‐ImDippN)Ti ( 1 ) in excellent yield. Upon standing in solution, 1 converts to a TiIV metallacycle ( 4 ) through dehydrogenation of a pendant isopropyl group. Spectroscopic evidence shows this transformation initially proceeds via the oxidative addition of a C(sp3)?H bond and can be reversed upon exposure of 4 to H2. Interestingly, treatment of 1 with cyclohexene gives cyclohexane and 4 via a titanium‐mediated transfer hydrogenation reaction, a process that can be extended to catalytically hydrogenate other unsaturated hydrocarbons under mild conditions. These results, rare for the early‐metals, suggest 1 possesses chemical characteristics reminiscent of noble, late‐metals.  相似文献   
6.
Fluorescent members of the 4, 4‐difluoro‐4‐bora‐3a, 4a‐diaza‐s‐indacene (BODIPY) family are widely used for a range of markers, dyes, and sensors. The capacity to substitute the basic framework is an attractive feature permitting a range of differently substituted materials to be formed. New isomeric BODIPYs, o‐, m‐, and p‐8‐[R‐C6H4]‐BODIPY (R = CH2OH, 2a (o), 2b (m), 2c (p); R = OMe, 3a (o), 3b (m), 3c (p)), have been synthesized and characterized by nuclear magnetic resonance, absorbance and emission spectroscopy, and single crystal X‐ray diffraction. The o‐isomers have a very high quantum yield emission in non‐polar solvents, while the m‐ and p‐ analogs showed weak fluorescence under the same conditions. Spectroscopic analysis, as well as X‐ray structural characterization, suggested that substitution in the ortho‐position of the phenyl ring is sufficient to increase the steric hindrance and hence impede the rotation of the phenyl moiety about the 8C‐C axis, thereby favoring radiative compared to non‐radiative relaxation. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   
7.
Given the unique structural and electronic properties of C60, metal–organic frameworks (MOFs) containing C60 linkers are expected to exhibit interesting characteristics. A new hexakisfullerene derivative possessing two pairs of phenyl pyridine groups attached to two methano‐carbon atoms located at the trans‐1 positions was designed and synthesized. The four pyridyl nitrogen atoms define a perfectly planar rectangle. This new C60 derivative was used to assemble the first fullerene‐linked two‐dimensional MOF by coordination with Cd2+.  相似文献   
8.
The synthesis and characterization of selenium‐containing stannanes, (o‐MeSeC6H4CH2)Sn(Ph)3–nCln [n = 0 ( 1Se ); 1 ( 2Se ); 2 ( 3Se )], is presented. The increasing Lewis acidity at tin in the series 1Se → 2Se → 3Se is reflected in their respective solid state arrangements and supramolecular architecture by interactions of the type Se ··· Se, Sn ··· Se, and Cl ··· H–C. Overall the capacity of the selenium atom to form bidentate interactions creates geometric assemblies distinctly different to those of the oxygen and sulfur analogs.  相似文献   
9.
The uses of low cost, renewable, environmentally friendly chitosan biopolymer as the structural template to control the size of silica particles in the range of nanometer scales are attractive for their practical industrial applications. In this paper, the nanostructured silica was synthesized using sodium silicate as the silica source and chitosan as the template under mild conditions. Effects of chitosan/silica ratio and aging temperature on the formation and the control of nanostructured silica was investigated by using thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), N2-sorption measurement, and transmission electron microscopy (TEM). It was found that the silica products were composed of the aggregates of primary silica nanoparticles and nanostructured silica units. At low aging temperature, the size of nanostructured silica was decreased when increasing the chitosan/silica ratio from 0.1 to 0.4. In contrast, the reverse trend was observed at the chitosan/silica ratio of higher than 0.4. The increase of aging temperature led to the formation of larger primary silica nanoparticles and nanostructured silica, and also promoted the formation of silica/chitosan composites. The fractal dimension calculated using modified FHH method found the linear correlation at two different regimes which might reflect the aggregates of silica products at different length scales.  相似文献   
10.
Different cyclo‐β‐dipeptides were prepared from corresponding N‐substituted β‐alanine derivatives under mild conditions using PhPOCl2 as activating agent in benzene and Et3N as base. To evaluate β3‐substituent influence, the amino acids 7 – 26 were synthesized, and a β‐lactam formation reaction was carried out instead of cyclo‐β‐dipeptide formation. The crystal structures of three derivatives of cyclo‐β‐peptides and one β‐lactam are presented.  相似文献   
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