Synthesis of 2-butyl-4,9-decadienoic and 2-butyl-4,9-dimethyl-4,9-decadienoic acids,structural analogues of cygerol

2-Butyl-4,9-decadienoic and 2-butyl-4,9-dimethyl-4,9-decadienoic acids, structural isomers of 2-cyclohexylgeranylacetic acid, which is an active component of the wound healing ointment cygerol, have been synthesized. Hydrocarbon chains C₁₀ have been obtained by the one-pot method of formation of long-chain hydrocarbons, namely, by the telomerization reaction of 1,3-dienes with nucleophiles catalyzed by palladium complexes. A heterogeneous palladium-zeolite catalyst has been used for the first time in telomerization of isoprene with piperidine.     

Trends in formation of the nanocrystalline structure and cationic ordering in the Dy2O3-HfO2 (1: 1) system

Evolution of the nanocrystalline structure of the complex oxide Dy₂HfO₅ in the course of thermal annealing at temperatures to 1600°C has been studied by a combination of X-ray and synchrotron methods, including traditional and anomalous X-ray diffraction, PDF, EXAFS, and SAXS. The changes in crystallite size upon annealing of the as-synthesized amorphous precursor have been analyzed in detail. The systematic distortions of a fluorite-type perfect crystal structure (space group $Fm\bar 3m$ ) related to the nonequivalence of the local environment of the Dy and Hf cations but not resulting in formation of a pyrochlore-type cationordered structure in this system have been examined.     

Complex Study of the Spearhead Superficial Crust from Burial Mound no. 1 near Novosvobodnaya Village

A complex study of a spearhead dated back to IV mill. BC from burial mound no. 1 near Novosvobodnaya village (collection of the State Historical Museum) and, in particular, the material of spearhead superficial crust has been performed. The elemental and phase composition of the metal of spearhead and the superficial crust on its surface have been determined by scanning electron microscopy, jointly with energydispersive X-ray microanalysis and X-ray phase analysis. A comparative analysis of the results of studying the spearhead superficial crust and similar crusts on other artifacts from the mounds near Novosvobodnaya village suggest natural origin of the crust on copper?arsenic artifacts.

     

Cluster-Type Structure of Amorphous Smooth Hydrocarbon CD<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> Films (<Emphasis Type="Italic">x</Emphasis> ~ 0.5) from T-10 Tokamak

Structure of smooth hydrocarbon CD _x films with a high deuterium ratio x ~ 0.5 redeposited from T-10 tokamak D-plasma discharges (NRC Kurchatov Institute, Moscow) has been studied. For the first time, small and wide angle X-ray scattering technique using synchrotron radiation and neutron diffraction have been employed. A fractal structure of CD _x films is found to consist of mass-fractals with rough border, surface fractals (with rough surface), plane scatterers and linear chains forming a branched and highly cross-linked 3D carbon network. The found fractals, including sp² clusters, are of typical size ~1.60 nm. They include a C₁₃ fragment consisting of three interconnected aromatic rings forming a minimal fractal sp² aggregate 9 × C₁₃. These graphene-like sp² clusters are interconnected and form a 3D lattice which can be alternatively interpreted as a highly defective graphene layer with a large concentration of vacancies. The unsaturated chemical bonds are filled with D, H atoms, linear sp² C=C, C=O, and sp³ structural elements like C-C, C-H(D), C-D_2,3, C-O, O-H, COOH, C _x D(H) _y found earlier from the infrared spectra of CD _x films, which are binding linear elements of a carbon network. The amorphous structure of CD _x films has been confirmed by the results of earlier fractal structure modeling, as well as by researches with X-ray photoelectron spectroscopy which allow finding a definite similarity with the electron structure of their model analogues — polymeric a-C:H and a-C:D films with a disordered carbon network consisting of atoms in sp³ + sp² states.     

Porosity and structural parameters of Karelian shungites according to the data of small-angle synchrotron radiation scattering and microscopy

The nanoporosity and structure of natural carbons has been investigated on the example of Karelian carbon-rich shungites by comparing the data of small-angle synchrotron radiation scattering and highresolution microscopy. The analysis of small-angle scattering data is based on the model of scattering spheres with lognormal size distribution. It is found that the structure of samples from the Maksovo and Zazhogino deposits subjected to high temperatures in the geological medium and (also to a lesser extent) a sample from the Shunga deposit can be described as an aggregation of polydisperse scattering spheres with lognormal size distribution; the characteristic scatterer size is determined for them. A comparison with microscopy data shows that these scatterers are mainly associated with pores, and the character of their size distribution is similar to that previously established for nanoglobules in schungites.     

Investigation of PdZn nanoparticle formation upon the thermal decomposition of acetate precursors by in situ XRD and XAFS

The formation of metal or metal-oxide nanoparticles from four different precursor systems, including palladium(II) acetate, zinc(II) acetate, their 1: 1 mechanical mixture and the palladium-zinc bimetallic acetate complex PdZn(OCOMe)₄(H₂O), upon heating in a He + 5% H₂ atmosphere is studied using the X-ray diffraction and EXAFS (Extended X-ray absorption fine structure) techniques in the in situ mode. X-ray diffraction is primarily used to monitor changes in the phase composition of the samples. At specific moments when qualitative changes in the composition occur, EXAFS spectra at the K-edges of Pd and Zn are also measured. Using a combination of these two techniques, a detailed sequence of the phase transformations in each of the four precursor systems is revealed. It is found that the bimetallic acetate complex and the mixture of two monometallic acetates undergo chemical reduction to form zerovalent palladium under milder conditions than zinc acetate. However, the formation of a PdZn alloy from the mixture of metal acetates proceeds with a significant diffusion barrier.     

A structural study of biocompatible magnetic nanofluid with synchrotron radiation-based X-ray scattering techniques

In this paper, water colloidal solutions of nanoparticles of magnetite (magnetic nanofluids, (MNFs)) are investigated by synchrotron X-ray diffraction (XRD) and small-angle scattering (SAXS). To prevent aggregation, nanoparticles are coated with polyacrylic acid (PAA) in a single solution and citric (CA) in the other solutions. In both cases, the maxima of the particle size distribution from SAXS (9?C10 nm) correspond to the sizes of the magnetite crystallites that were estimated from the broadening of the diffraction lines. In addition, the SAXS data indicate the presence of a significant proportion of aggregates (up to 60 nm in diameter) in both colloidal solutions, although fundamental differences in the structures of aggregates between the MNFs stabilized by PAA and CA were not observed. In this study determination of the structural characteristics of MNFs were carried out in order to obtain stable dispersive non-aggregating nanoparticles of magnetite for use as contrast agents in magnetic resonance tomography, drug carriers, and other biomedical applications.     

Study of Bronze Statues “John the Baptist” and “Dancing Cupid” from the Collections of the Pushkin State Museum

Crystallography Reports - Bronze statues “John the Baptist” and “Dancing Cupid” from the collections of the Pushkin State Museum of Fine Arts have been investigated at the...     

Magnetodielectric composites based on functionalized polyphenylene sulfides containing iron nanoparticles

Preparation of iron-filled polyaminophenylene sulfides and polyhydroxyaminophenylene sulfides by the metal vapor procedure was studied. Nanocomposites based on these metal-containing polymers and epoxy-isopropylidenediphenol oligomers (ED-20) were prepared and their composition, properties, and structure were studied by X-ray diffraction and thermogravimetric analyses, and thermomechanical methods. The magnetic and dielectric properties of the materials were determined.