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1.
Science ; 355(6321): 166-169, 2017 01 13.
Article in English | MEDLINE | ID: mdl-28082587

ABSTRACT

The localization of hydrogen atoms is an essential part of crystal structure analysis, but it is difficult because of their small scattering power. We report the direct localization of hydrogen atoms in nanocrystalline materials, achieved using the recently developed approach of dynamical refinement of precession electron diffraction tomography data. We used this method to locate hydrogen atoms in both an organic (paracetamol) and an inorganic (framework cobalt aluminophosphate) material. The results demonstrate that the technique can reliably reveal fine structural details, including the positions of hydrogen atoms in single crystals with micro- to nanosized dimensions.

2.
Nanoscale ; 6(18): 10859-64, 2014 Sep 21.
Article in English | MEDLINE | ID: mdl-25117582

ABSTRACT

The preparation of pure zeolite nanocrystals (EMT-type framework) and their silver ion-exchanged (Ag(+)-EMT) and reduced silver (Ag(0)-EMT) forms is reported. The template-free zeolite nanocrystals are stabilized in water suspensions and used directly for silver ion-exchange and subsequent chemical reduction under microwave irradiation. The high porosity, low Si/Al ratio, high concentration of sodium and ultrasmall crystal size of the EMT-type zeolite permitted the introduction of a high amount of silver using short ion-exchange times in the range of 2-6 h. The killing efficacy of pure EMT, Ag(+)-EMT and Ag(0)-EMT against Escherichia coli was studied semi-quantitatively. The antibacterial activity increased with increasing Ag content for both types of samples (Ag(+)-EMT and Ag(0)-EMT). The Ag(0)-EMT samples show slightly enhanced antimicrobial efficacy compared to that of Ag(+)-EMT, however, the differences are not substantial and the preparation of Ag nanoparticles is not viable considering the complexity of preparation steps.


Subject(s)
Anti-Bacterial Agents/chemistry , Nanoparticles/chemistry , Silver/chemistry , Zeolites/chemistry , Anti-Bacterial Agents/pharmacology , Escherichia coli/drug effects
3.
J Inorg Biochem ; 105(11): 1391-7, 2011 Nov.
Article in English | MEDLINE | ID: mdl-21946439

ABSTRACT

A family of tripodal pyrazole-based ligands has been synthesized by a condensation reaction between 1-hydroxypyrazoles and aminoalcohols. The diversity was introduced both on the substituents of the pyrazole ring and on the side chain. The corresponding copper(II) complexes have been prepared by reaction with CuCl(2) in tetrahydrofuran. They have been characterized by EPR, UV spectroscopy and cyclic voltammetry. The absence of the half-field splitting signals in EPR suggests that the complex exists in solution as mononuclear species. The influence of substituents and side chain of the tripodal ligand on the catecholase activity of the complexes was studied. The reaction rate depends on two factors. First, the presence of an oxygen atom in the third position of the side chain should be avoided to keep the effectiveness of the reaction. Second, the electronic and steric effects of substituents on the pyrazole ring strongly affect the catalytic activity of the complex. Thus, best results were obtained with complexes containing unsubstituted pyrazole based-ligands. Kinetic investigations with the best catalyst based on the Michaelis-Menten model show that the catalytic activity of the mononuclear complex is close to that of some dicopper complexes described in literature.


Subject(s)
Catechols/chemistry , Coordination Complexes/chemical synthesis , Copper/chemistry , Pyrazoles/chemical synthesis , Biomimetics , Catalysis , Chelating Agents , Coordination Complexes/chemistry , Electrochemistry , Electron Spin Resonance Spectroscopy , Hydrogen Peroxide/chemistry , Kinetics , Oxidation-Reduction , Pyrazoles/chemistry , Spectrophotometry, Ultraviolet
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