Strategies for collecting screen-less oscillation data

Screen-less oscillation photography is the method of choice for recording three-dimensional X-ray diffraction data for crystals of biological macromolecules. The geometry of an oscillation camera is extremely simple. However, the manner in which the reciprocal lattice is recorded in any experiment is fairly complex. This depends on the Laue symmetry of the reciprocal lattice, the lattice type, the orientation of the crystal on the camera and to a lesser extent on the unit-cell dimensions. Exploring the relative efficiency of collecting X-ray diffraction data for different crystal orientations prior to data collection might reduce the number of films required to record most of the unique data and the consequent amount of time required for processing these films. Here algorithms are presented suitable for this purpose and results are reported for the 11 Laue groups, different lattice types and crystal orientations often employed in data collection.

Study on the pH dependence of diffraction efficiency of phase holograms in dye sensitized dichromated gelatin

Dichromated gelatin is thought to be a good substitute for photographic emulsions in some uses. The results of a systematic study of the effect of the pH of the developer on the diffraction efficiency of volume holographic gratings recorded in dye sensitized dichromated gelatin are presented.

A neutron diffraction investigation of the structure of PBO-PBCL2 glasses

Neutron diffraction techniques have been employed to investigate the structure of PbO-PbCl2 glasses as a function of composition in the nominal range PbO.PbCl2 to 9PbO.PbCl2. It is concluded that, whereas the first Pb-O distance is well defined, the distribution of Pb-Cl distances is much broader, in agreement with a previous EXAFS study.

A need for re-examination of the fibre diffraction data of A-DNA

A-DNA pattern, obtained using a flat plat camera, was indexed by Fuller Image on the basis of a c-face centred monoclinic cell with A = 22.24 Å, B = 40.62 Å, C = 28.15 Å and β = 97.0°. A precession photograph of A-DNA which gives an undistorted picture of the lattice, showed that the unit cell parameters as given by Fuller Image were not quite correct. The precession photograph showed a strong meridional reflection (R = 0.00 Å−1) on the 11th layer line. But the occurrence of the meridional reflection on the 11th layer line could not be explained on the basis of the cell parameters given by Fuller Image ; using those cell parameters the reflection which comes closest to the meridian on 11th layer line is at R = 0.025 Å−1. However, a simple interchange of a and b values accounted for the meridional reflection on 11th layer line. The corrected cell parameter refined against 28 strong spots are A = 40.75 Å, B = 22.07 Å, C = 28.16 Å and β = 97.5°. In the new unit cell of A-DNA, the packing arrangement of the two molecules is different from that in the old one. Nonetheless, our earlier contention is again reaffirmed that both right and left-handed A-DNA are stereochemically allowed and consistent with the observed fibre pattern.

Crystal Physics, Diffraction, Theoretical and General Crystallography

A formula has been derived for the mean-square error in the phases of crystal reflections determined through the multiwavelength anomalous scattering method. The error is written in terms of a simple function of the positions in the complex plane of the 'centres' corresponding to the different wavelengths. For the case of three centres, the mean-square error is inversely proportional to the area of the triangle formed by them. The theoretical values are in good agreement with those obtained by earlier workers from computer simulations. The present method makes it easier to optimize the number and the actual wavelengths to be employed in the multiwavelength method. The maximum benefits of this method are expected in experiments employing synchrotron radiation or neutrons.

Neutron-diffraction study of structure and conformation of nucleotide uridine-5 phosphate (disodium salt)

Acta Crystallographica Section A: Foundations of Crystallography covers theoretical and fundamental aspects of the structure of matter. The journal is the prime forum for research in diffraction physics and the theory of crystallographic structure determination by diffraction methods using X-rays, neutrons and electrons. The structures include periodic and aperiodic crystals, and non-periodic disordered materials, and the corresponding Bragg, satellite and diffuse scattering, thermal motion and symmetry aspects. Spatial resolutions range from the subatomic domain in charge-density studies to nanodimensional imperfections such as dislocations and twin walls. The chemistry encompasses metals, alloys, and inorganic, organic and biological materials. Structure prediction and properties such as the theory of phase transformations are also covered.

The nonplanar peptide unit III. Quantum chemical calculations for related compounds and experimental X-ray diffraction data

The possible nonplanar distortions of the amide group in formamide, acetamide, N-methylacetamide, and N-ethylacetamide have been examined using CNDO/2 and INDO methods. The predictions from these methods are compared with the results obtained from X-ray and neutron diffraction studies on crystals of small open peptides, cyclic peptides, and amides. It is shown that the INDO results are in good agreement with observations, and that the dihedral angles N and defining the nonplanarity of the amide unit are correlated approximately by the relation N = -2, while C is small and uncorrelated with . The present study indicates that the nonplanar distortions at the nitrogen atom of the peptide unit may have to be taken into consideration, in addition to the variation in the dihedral angles (,), in working out polypeptide and protein structures.

A note on Sommerfeld's diffraction problem

A direct transform technique is found to be most suitable for attacking two-dimensional diffraction problems. As a first example of the application of the technique, the well-known Sommerfeld problem is reconsidered and the solution of the problem of diffraction, by a half-plane, of a cylindrical pulse is made use of in deducing the solution of the problem of diffraction of a plane wave by a soft half-plane. Journal of Mathematical Physics is copyrighted by The American Institute of Physics.

Apparent shortening of the Csp(3)-Csp(3) bond analysed via a variable-temperature X-ray diffraction study in racemic 1,1 '-binaphthalene-2,2 '-diyl diethyl bis(carbonate)

Crystal structure determination at room temperature [292 (2) K] of racemic 1,1'-binaphthalene-2,2'-diyl diethyl bis(carbonate), C26H22O6, showed that one of the terminal carbon-carbon bond lengths is very short [Csp(3)-Csp(3) = 1.327 (6) angstrom]. The reason for such a short bond length has been analysed by collecting data sets on the same crystal at 393, 150 and 90 K. The values of the corrected bond lengths clearly suggest that the shortening is mainly due to positional disorder at two sites, with minor perturbations arising as a result of thermal vibrations. The positional disorder has been resolved in the analysis of the 90 K data following the changes in the unit-cell parameters for the data sets at 150 and 90 K, which appear to be an artifact of a near centre of symmetry relationship between the two independent molecules in the space group P (1) over bar at these temperatures. Indeed, the unit cell at low temperature (150 and 90 K) is a supercell of the room-temperature unit cell.

Systematic study on crystal-contact engineering of diphthine synthase: influence of mutations at crystal-packing regions on X-ray diffraction quality

It is well known that protein crystallizability can be influenced by site-directed mutagenesis of residues on the molecular surface of proteins, indicating that the intermolecular interactions in crystal-packing regions may play a crucial role in the structural regularity at atomic resolution of protein crystals. Here, a systematic examination was made of the improvement in the diffraction resolution of protein crystals on introducing a single mutation of a crystal-packing residue in order to provide more favourable packing interactions, using diphthine synthase from Pyrococcus horikoshii OT3 as a model system. All of a total of 21 designed mutants at 13 different crystal-packing residues yielded almost isomorphous crystals from the same crystallization conditions as those used for the wild-type crystals, which diffracted X-rays to 2.1 angstrom resolution. Of the 21 mutants, eight provided crystals with an improved resolution of 1.8 angstrom or better. Thus, it has been clarified that crystal quality can be improved by introducing a suitable single mutation of a crystal-packing residue. In the improved crystals, more intimate crystal-packing interactions than those in the wild-type crystal are observed. Notably, the mutants K49R and T146R yielded crystals with outstandingly improved resolutions of 1.5 and 1.6 angstrom, respectively, in which a large-scale rearrangement of packing interactions was unexpectedly observed despite the retention of the same isomorphous crystal form. In contrast, the mutants that provided results that were in good agreement with the designed putative structures tended to achieve only moderate improvements in resolution of up to 1.75 angstrom. These results suggest a difficulty in the rational prediction of highly effective mutations in crystal engineering.

Unraveling the packing pattern leading to gelation using SS NMR and X-ray diffraction: direct observation of the evolution of self-assembled fibers

A detailed understanding of the mode of packing patterns that leads to the gelation of low molecular mass gelators derived from bile acid esters was carried out using solid state NMR along with complementary techniques such as powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and polarizing optical microscopy (POM). Solid state C-13{H-1} cross polarization (CP) magic angle spinning (MAS) NMR of the low molecularmass gel in its native state was recorded for the first time. A close resemblance in the packing patterns of the gel, xerogel and bulk solid states was revealed upon comparing their C-13{H-1} CPMAS NMR spectral pattern. A doublet resonance pattern of C-13 signals in C-13{H-1}CPMAS NMR spectra were observed for the gelator molecules, whereas the non-gelators showed simple singlet resonance or resulted inthe formation of inclusion complexes/solvates. PXRD patterns revealed a close isomorphous nature of the gelators indicating the similarity in the mode of the packing pattern in their solid state. Direct imaging of the evolution of nanofibers (sol-gel transition) was carried out using POM, which proved the presence of self-assembled fibrillar networks (SAFINs) in the gel. Finally powder X-ray structure determination revealed the presence of two non-equivalent molecules in an asymmetric unit which is responsible for the doublet resonance pattern in the solid state NMR spectra.

An electron diffraction investigation of the molecular structure of methyl azide

The molecular structure of methyl azide has been studied by the sector-microphotometer and the sector-visual methods of electron diffraction and the parameters determined as follows: C-N = 1.47 ± 0.02 Å., N1-N2 = 1.24 ± 0.01 Å., N2-N3 = 1.12 ± 0.01 Å. and

An electron diffraction investigation of the molecular structure of trichloroacetonitrile

The molecular structure of trichloroacetonitrile has been studied by electron diffraction by the visual interpretation of sectored photographs. These parameters were obtained: C-N = 1.165 ± 0.025, C-C = 1.465 ± 0.025, C-Cl = 1.765 ± 0.01 A., and < CCCl = 109.5 ± 1°.

Electron diffraction patterns from the Al-Mn decagonal phase

The variety of electron diffraction patterns arising from the decagonal phase has been explored using a stereographic analysis for generating the important zone axes as intersection points corresponding to important relvectors. An indexing scheme employing a set of five vectors and an orthogonal vector has been followed. A systematic tilting from the decagonal axis to one of the twofold axes has been adopted to generate a set of experimental diffraction patterns corresponding to the expected patterns from the stereographic analysis with excellent agreement.