Diffraction experiments X-ray

Illuminating the sample at grazing angles. The penetration depth of photons depends on the cosine of the incidence angle and, therefore, can be reduced by this procedure. Although such an approach has limited use, it has been successfully employed in a few instances, such as for x-ray diffraction experiments. 

The transition from smectic A to smectic B phase is characterized by tire development of a sixfold modulation of density witliin tire smectic layers ( hexatic ordering), which can be seen from x-ray diffraction experiments where a sixfold symmetry of diffuse scattering appears. This sixfold symmetry reflects tire bond orientational order. An appropriate order parameter to describe tlie SmA-SmB phase transition is tlien [18,19 and 20]... 

Apart from the sheer complexity of the static stmctures of biomolecules, they are also rather labile. On the one hand this means that especial consideration must be given to the fact (for example in electron microscopy) that samples have to be dried, possibly stained, and then measured in high vacuum, which may introduce artifacts into the observed images [5]. On the other, apart from the vexing question of whether a protein in a crystal has the same stmcture as one freely diffusing in solution, the static stmcture resulting from an x-ray diffraction experiment gives few clues to the molecular motions on which operation of an enzyme depends [6]. 

Zeolites and Catalytic Cracking. The best-understood metal oxide catalysts are zeoHtes, ie, crystalline aluminosihcates (77—79). The zeoHtes are well understood because they have much more nearly uniform compositions and stmctures than amorphous metal oxides such as siUca and alumina. Here the usage of amorphous refers to results of x-ray diffraction experiments the crystaUites of a metal oxide such as y-Al202 that constitute the microparticles are usually so small that sharp x-ray diffraction patterns are not measured consequendy the soHds are said to be x-ray amorphous or simply amorphous. 

In an x-ray diffraction experiment on a single crystal of sodium chloride, with the use of radiation from a copper source (X = 154 pm), constructive interference was observed at 0 = 11.2°. What is the spacing of the layers responsible for the diffraction ... 

Electron microscopy and X-ray diffraction experiments conducted on resilin-containing insect cuticle provided further support for resilin existing in the rubbery state as a crosslinked random network of protein chains. No fine structure was revealed by the electron microscopy experiments and zero crystallinity could be detected from the X-ray diffraction experiments. Furthermore, the diffraction... 

X-ray diffraction experiments revealed a psendo-cubic orthorombic unit cell with cell dimensions similar to the expected cubic F centered arrangement of the predesigned diamond-like crystal. 

Figure 1. Time-resolved X-ray diffraction experiment (schematic). The liquid sample is excited by a laser pulse, and its temporal evolution is monitored by a time-delayed X-ray pulse. The diffracted radiation is measured by a charge-coupled detector (CCD). In practice, the laser and X-ray beams are not perpendicular to each other, but nearly parallel.

Gas-phase methylation of catechol by methanol was studied on y -AI2O3 modified by the basic elements K, Li, Mg and Ca. Addition of 7.5 at.% Mg to y-AljOa was optimal and increased the 3-methyl catechol selectivity from 0.26 to 0.65. X-ray diffraction experiments showed the diffusion of Li and Mg cations into the y -AI2O3 bulk. This induces a change in the surface species (XPS data) and the surface acid-base properties (TPD experiments). Ca and K addition to y-alumina was ineffective due to formation of basic oxide layers on the sur ce. 

Since optical measurements of monolayers at the water-oil interface are rather difficult to carry out, a configuration was suggested where a monolayer at the water-air interface was in contact with an oil lens which was partly wetting the monolayer [23]. The thermodynamic relation between this monolayer and that residing at the water-oil interface was discussed. This configuration was utilized in the X-ray diffraction experiments [24] where the structural changes of dipalmitoyl phosphatidylcholine (DPPC) and DPPE were followed. 

The shortest cation-anion distance in an ionic compound corresponds to the sum of the ionic radii. This distance can be determined experimentally. However, there is no straightforward way to obtain values for the radii themselves. Data taken from carefully performed X-ray diffraction experiments allow the calculation of the electron density in the crystal the point having the minimum electron density along the connection line between a cation and an adjacent anion can be taken as the contact point of the ions. As shown in the example of sodium fluoride in Fig. 6.1, the ions in the crystal show certain deviations from spherical shape, i.e. the electron shell is polarized. This indicates the presence of some degree of covalent bonding, which can be interpreted as a partial backflow of electron density from the anion to the cation. The electron density minimum therefore does not necessarily represent the ideal place for the limit between cation and anion. 

The advent of CCD detectors for X-ray diffraction experiments has raised the possibility of obtaining charge density data sets in a much reduced time compared to that required with traditional point detectors. This opens the door to many more studies and, in particular, comparative studies. In addition, the length of data collection no longer scales with the size of the problem, thus the size of tractable studies has certainly increased but the limit remains unknown. Before embracing this new technology, it is necessary to evaluate the quality of the data obtained and the possible new sources of error. The details of the work summarized below has either been published or submitted for publication elsewhere [1-3]. 

Table 1. LR-B/081 crystal data and summary of the X-ray diffraction experiment. 

For the crystalline materials, high resolution X-ray diffraction experiment is a powerful tool to derive accurate electron density even for large systems like zeolites. In this study, we are interested in the experimental electron density distribution in the scolecite CaAl2Si3O10 3H20 in order to make comparison with its sodium analogue natrolite Na2Al2Si3Oi0 2H20 for which the electron density has been reported recently [1,2],... 

According to [98,99], the compound Tc2O3[C5(CH3)5 n has a polymeric structure with R(Tc-Tc) = 1.867(4) A. However, these authors do not report the details of the X-ray diffraction experiment and the atomic coordinates. Therefore, these data seem doubtful. 

In the paramagnetic regime, the evolution of the EPR line width and g value show the presence of two transitions, observed at 142 and 61 K in the Mo salt, and at 222 and 46 K in the W salt. Based on detailed X-ray diffraction experiments performed on the Mo salt, the high temperature transition has been attributed to a structural second-order phase transition to a triclinic unit cell with apparition of a superstructure with a modulation vector q = (0,1/2, 1/2). Because of a twinning of the crystals at this transition, it has not been possible to determine the microscopic features of the transition, which is probably associated to an ordering of the anions, which are disordered at room temperature, an original feature for such centrosymmetric anions. This superstructure remains present down to the Neel... 

In this paper, UV-visible absorption spectra and X-ray diffraction experiments of single crystals and solvent cast films of the azobenzene amphiphiles, CnAzoCmN+Br, were systematically investigated. Structural characterization of the cast bilayer films are discussed in comparison with aqueous solutions and single crystals. Some novel functional properties of the cast films are described, too. We also emphasize that the two-dimensional molecular assemblies, cast films and crystals of bilayer-forming amphiphiles, are suitable candidates for "crystal engineering" because of their simple structures compared with usual three-dimensional molecular crystals. 

Table II. Long periods (nm) of cast films calculated from X-ray diffraction experiment.

Equation (2) indicates that an increase of the tilt angle from 26° to 36° results a small blue shift of the absorption maximum (in wavelength) in the visible region. Spectral observation of the group VI (375 nm) and V (360 nm) is very consistent with the structural estimation from the X-ray diffraction experiments. 

Since polymer single crystals prepared these days are too small for x-ray diffraction experiments, the Crystal Structure of a polymer is generally determined from x-ray patterns of a fibre drawn from the polymer. Due to the alignment of the crystalline regions with the long axes of the molecules parallel to the fibre axis, the pattern is essentially identical to a rotation pattern from... 

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