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.

a b s t r a c tThis article outlines the importance of zeolite synthesis and their unique physicochemical characteristics promoting advanced applications. The main strategies for preparation of zeolites including organic-template assisted, organic-template free and alternative procedures are considered for synthesis of crystallites offering control and fine-tuning of their properties. Besides, rational design of zeolites with pre-determined structure, porosity, size, morphology, and composition are more viable by studying carefully the chemical and physical parameters controlling the zeolite synthesis and understanding the crystallization mechanism. Finally, a particular attention to the preparation of zeolites with nanosized dimensions and their utilization in innovative applications including photovoltaic, medicine and holographic sensors are presented.

The synthesis, luminescence, and nonlinear optical properties of a new series of Ir(ppy)3 (ppy = 2-phenylpyridine) complexes incorporating π-extended vinyl-aryl substituents at the para positions of their pyridine rings are reported. Appropriate substitution of the pyridyl rings allows the tuning of the luminescence properties and the second-order nonlinear optical response of this unusual family of three-dimensional chromophores. Theoretical calculations were performed to evaluate the dipole moments, to gain insight into the electronic structure, and to rationalize the observed optical properties of the investigated complexes.

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.

A facile and rapid photochemical method for preparing supported silver nanoparticles (Ag-NPs) in a suspension of faujasite type (FAU) zeolite nanocrystals is described. Silver cations are introduced by ion exchange into the zeolite and subsequently irradiated with a Xe-Hg lamp (200 W) in the presence of a photoactive reducing agent (2-hydroxy-2-methylpropiophenone). UV-vis characterization indicates that irradiation time and intensity (I0) influence significantly the amount of silver cations reduced. The full reduction of silver cations takes place after 60 s of a polychromatic irradiation, and a plasmon band of Ag-NPs appears at 380 nm. Transmission electron microscopy combined with theoretical calculation of the plasmon absorbance band using Mie theory shows that the Ag-NPs, stabilized in the micropores and on the external surface of the FAU zeolite nanocrystals, have an almost spheroidal shape with diameters of 0.75 and 1.12 nm, respectively. Ag-NPs, with a homogeneous distribution of size and morphology, embedded in a suspension of FAU zeolites are very stable (∼8 months), even without stabilizers or capping agents.

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The host-guest and guest-guest interactions governing the CO 2 adsorption/desorption in two nanosized zeolite samples with FAU framework type and different Si/Al ratios (Na-X Si/Al=1.24 and Na-Y Si/Al=2.54) and cations distribution were investigated by in situ synchrotron high resolution X-ray powder diffraction (XRPD) and in situ FTIR spectroscopy. The two complementary techniques allow probing the CO 2 adsorption/desorption in the FAU zeolites at different levels, i.e. average structure by XRPD vs local structure by IR. The presence of physisorbed CO 2 molecules in both zeolites was detected by XRPD, while only a high amount of chemisorbed CO 2 in the Na-X zeolite was found. The presence of unshielded Na cations and H 2 O molecules in the supercage of the Na-X sample induces the formation of stable bidentate bicarbonate groups. The evacuating of CO 2 loaded samples resulted in an efficient removal of physisorbed CO 2 from both nanosized zeolites, on the contrary high temperature is required to remove the chemisorbed species from the nanosized Na-X zeolite. Understanding the CO 2 sorption behavior and capacity of nanosized zeolites is of great importance in broadening their use in environmental, clinical and biomedical applications.

Palladium-catalysed direct 5-arylation of metallated thiophenes of fac-Ir(N^C(3')-thpy)(3) with aryl bromides via C-H bond functionalisation allows the synthesis of a variety of new Ir complexes in only one step (thpyH = 2,2'-thienylpyridine). The method offers simple modification of the nature of the ligand and hence of the photophysical properties of such complexes.