scholarly journals Concerning Single Crystal Reflectivity Curves

1988 ◽  
Vol 41 (3) ◽  
pp. 393
Author(s):  
A McL Mathieson
Keyword(s):  
Single Crystal ◽  
Experimental Evidence ◽  
Structure Factor ◽  
Bragg Reflection ◽  
Half Maximum ◽  
Reflectivity Curve ◽  
One Dimensional ◽  
Structure Factors ◽  
Kinematical Limit

The extinguished reflectivity curve of a Bragg single crystal reflection represents the basic experimental evidence for the determination of accurate structure factors. In normal measurement procedures of one-dimensional (ID) 'counter' profiles, information on such curves is obscured by the presence of other, more dominant components. It is therefore difficult to separate out these curves so that a realistic correction for extinction can be applied. By considering the 'shape' of a Bragg reflection in the plane of diffraction from the ~w, ~2e viewpoint, procedures have been deduced for practical zero wavelength dispersion measurement of reflectivity curves for virtually any e value and, with these curves, corrections can be applied to produce extinction-free structure factor values. Attention is drawn to the fact that the width of the experimental reflectivity curve (say at half maximum) can provide a valuable criterion to assist in attaining the 'kinematical limit'.

scholarly journals Simple Method for Estimating the Contribution of Neighbouring n-beam Interactions to Two-beam Structure Factors

1988 ◽  
Vol 41 (3) ◽  
pp. 469
Author(s):  
HJ Juretschke ◽  
HK Wagenfeld
Keyword(s):  
Experimental Determination ◽  
Structure Factor ◽  
Beam Structure ◽  
Simple Method ◽  
Experimental Configuration ◽  
Structure Factors ◽  
Special Cases ◽  
Better Than

Unless special precautions are taken, the experimental determination of two-beam structure factors to better than 1 % may include contributions from neighbouring n-beam interactions. In any particular experimental configuration, corrections for such contributions are easily carried out using the modified two-beam structure factor formalism developed recently (Juretschke 1984), once the full indexing of the pertinent n-beam interactions is known. The method is illustrated for both weak and strong primary reflections and its applicability in special cases, as well as for less than perfect crystals, is discussed.

Obtaining the structure factors for an epitaxial film using Cu X-ray radiation

2013 ◽  
Vol 46 (6) ◽  
pp. 1749-1754 ◽  
Author(s):  
P. Wadley ◽  
A. Crespi ◽  
J. Gázquez ◽  
M.A. Roldán ◽  
P. García ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thin Films ◽  
Structure Factor ◽  
Tetragonal Symmetry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Structure Factors ◽  
Scanning Transmission

Determining atomic positions in thin films by X-ray diffraction is, at present, a task reserved for synchrotron facilities. Here an experimental method is presented which enables the determination of the structure factor amplitudes of thin films using laboratory-based equipment (Cu Kα radiation). This method was tested using an epitaxial 130 nm film of CuMnAs grown on top of a GaAs substrate, which unlike the orthorhombic bulk phase forms a crystal structure with tetragonal symmetry. From the set of structure factor moduli obtained by applying this method, the solution and refinement of the crystal structure of the film has been possible. The results are supported by consistent high-resolution scanning transmission electron microscopy and stoichiometry analyses.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXXIV Synthesis and Structure of the 1 : 1 Adduct of Silver(I) Nitrate with Triphenylstibine

1997 ◽  
Vol 50 (6) ◽  
pp. 671 ◽  
Author(s):  
Effendy ◽  
John D. Kildea ◽  
Allan H. White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Related Species ◽  
Room Temperature ◽  
Structural Data ◽  
Lewis Base ◽  
One Dimensional ◽  
X Ray ◽  
The One

The synthesis and room-temperature single-crystal X-ray structure determination of the 1 : 1 adduct of silver(I) nitrate with triphenylstibine, AgNO3/SbPh3 (1 : 1), is recorded, being monoclinic, Cc,a 12·824(2), b 15·794(4),c 9·796(2) Å, β 117·50(1)°, Z= 4; conventional R on F was 0·030 for 2881 independent ‘observed’ (I > 3σ(I)) reflections. The complex is a one-dimensional polymer with bridging nitrate groups, resembling in this respect its phosphine and arsine analogues. The completion of this study, along with related species recorded in accompanying papers, means that full structural data are now available for the complete array AgNO3/EPh3 (1 : n), E = P, As, Sb, n = 1–4, with the one exception of E = Sb, n = 2.

scholarly journals Accurate Determination of Structure Factors by Pendellosung Methods Using White Radiation

1988 ◽  
Vol 41 (3) ◽  
pp. 433 ◽  
Author(s):  
T Takama ◽  
S Sato
Keyword(s):  
Single Crystal ◽  
Accurate Determination ◽  
Diffraction Theory ◽  
Specimen Thickness ◽  
Dynamical Diffraction ◽  
Laue Spot ◽  
Exit Surface ◽  
Structure Factors ◽  
Integrated Intensity

This paper describes two experimental techniques measuring the Pendellosung beats using white radiation, developed in the authors' laboratory. The intensity of a Laue spot diffracted from a parallel-sided single crystal is successively measured at different Bragg angles, i.e. with different wavelengths. The values of structure factors are evaluated from extremum positions in the measured beats on the basis of the dynamical diffraction theory. In the first method, the integrated intensity diffracted from the whole exit surface is measured, and in the second, the measurement is made only at the centre of the Borrmann fan on the exit surface of a specimen. A discussion is given on the accuracy associated with the following origins of errors: (1) polarisation of incident white radiation, (2) measurement of specimen thickness, (3) measurement of wavelength, (4) determination of extremum positions, and (5) effect of defects in the crystal.

Time-of-flight Bragg scattering from aligned stacks of lipid bilayers using the Liquids Reflectometer at the Spallation Neutron Source

2012 ◽  
Vol 45 (6) ◽  
pp. 1219-1227 ◽  
Author(s):  
Jianjun Pan ◽  
Frederick A. Heberle ◽  
Justin R. Carmichael ◽  
John F. Ankner ◽  
John Katsaras
Keyword(s):  
Lipid Bilayers ◽  
Neutron Source ◽  
Scattering Length ◽  
Time Of Flight ◽  
Spallation Neutron Source ◽  
Bragg Scattering ◽  
One Dimensional ◽  
Structure Factors ◽  
The One

Time-of-flight (TOF) neutron diffraction experiments on aligned stacks of lipid bilayers using the horizontal Liquids Reflectometer at the Spallation Neutron Source are reported. Specific details are given regarding the instrumental setup, data collection and reduction, phase determination of the structure factors, and reconstruction of the one-dimensional neutron scattering length density (NSLD) profile. The validity of using TOF measurements to determine the one-dimensional NSLD profile is demonstrated by reproducing the results of two well known lipid bilayer structures. The method is then applied to show how an antimicrobial peptide affects membranes with and without cholesterol.

scholarly journals Use of Extinction Corrections in Neutron Diffraction Experiments

1988 ◽  
Vol 41 (3) ◽  
pp. 383 ◽  
Author(s):  
A Delapalme
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Experimental Evidence ◽  
Diffraction Data ◽  
Structure Factor ◽  
Lorentz Factor ◽  
Relative Importance ◽  
Diffraction Experiment ◽  
Neutron Diffraction Data ◽  
Neutron Diffraction Experiment

The study of extinction by neutrons reveals many features of the extinction problem: theory and practical cases, polarised and unpolarised neutron cases. Special attention is given to the usual extinction corrections for neutron diffraction experiments, showing the relative importance of structure factor, wavelength, Lorentz factor, mosaic and the path of neutrons through the crystal. Two problems are reviewed: (a) how to detect the presence of extinction in both cases of a single crystal experiment with polarised and unpolarised neutrons; and (b) after experimental evidence for extinction in a neutron diffraction experiment, how to follow a reliable way to correct the neutron diffraction data in both cases of polarised and unpolarised neutron experiments. Some examples are given.

Signal to noise considerations for single crystal femtosecond time resolved crystallography of the Photoactive Yellow Protein

2014 ◽  
Vol 171 ◽  
pp. 439-455 ◽  
Author(s):  
Jasper J. van Thor ◽  
Mark M. Warren ◽  
Craig N. Lincoln ◽  
Matthieu Chollet ◽  
Henrik Till Lemke ◽  
...  
Keyword(s):  
Single Crystal ◽  
Structure Factor ◽  
Bragg Reflection ◽  
Threshold Concentration ◽  
Photoactive Yellow Protein ◽  
Signal To Noise ◽  
Time Resolved ◽  
X Ray ◽  
Mosaic Spread ◽  
Rotation Method

Femtosecond time resolved pump–probe protein X-ray crystallography requires highly accurate measurements of the photoinduced structure factor amplitude differences. In the case of femtosecond photolysis of single P63crystals of the Photoactive Yellow Protein, it is shown that photochemical dynamics place a considerable restraint on the achievable time resolution due to the requirement to stretch and add second order dispersion in order to generate threshold concentration levels in the interaction region. Here, we report on using a ‘quasi-cw’ approach to use the rotation method with monochromatic radiation and 2 eV bandwidth at 9.465 keV at the Linac Coherent Light Source operated in SASE mode. A source of significant Bragg reflection intensity noise is identified from the combination of mode structure and jitter with very small mosaic spread of the crystals and very low convergence of the XFEL source. The accuracy with which the three dimensional reflection is approximated by the ‘quasi-cw’ rotation method with the pulsed source is modelled from the experimentally collected X-ray pulse intensities together with the measured rocking curves. This model is extended to predict merging statistics for recently demonstrated self seeded mode generated pulse train with improved stability, in addition to extrapolating to single crystal experiments with increased mosaic spread. The results show that the noise level can be adequately modelled in this manner, indicating that the large intensity fluctuations dominate the merged signal-to-noise (I/σI) value. Furthermore, these results predict that using the self seeded mode together with more mosaic crystals, sufficient accuracy may be obtained in order to resolve typical photoinduced structure factor amplitude differences, as taken from representative synchrotron results.

New procedure to obtain Bragg-reflection intensities from FULLPROF suite for powder crystal-structure determination using GEST and PECKCRYST programs

2010 ◽  
Vol 25 (4) ◽  
pp. 374-376
Author(s):  
Zhen Jie Feng ◽  
Yong Lei Zheng ◽  
Yu Ling Su ◽  
Biao Shao ◽  
Ming Tao Li ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Small Molecules ◽  
Powder Diffraction ◽  
Structure Determination ◽  
Bragg Reflection ◽  
Crystal Structure Determination ◽  
Diffraction Determination ◽  
Good Agreement

A useful procedure is described to rapidly obtain Bragg-reflection intensities from the FULLPROF suite, and the Bragg intensities can then be input into the GEST and the PECKCRYST programs for crystal-structure determination of small molecules. An example on using the new procedure for the structure determination from powder diffraction determination of hydrochlorothiazide (C7H8ClN3O4S2) is presented, and the powder-structure results obtained by the PECKCRYST program are in good agreement with previously reported single-crystal results.

scholarly journals Non-systematic Three-beam Effects in Dynamical Electron Diffraction and Their Use in Determination of Amplitude and Phase of Structure Factors

1988 ◽  
Vol 41 (3) ◽  
pp. 449 ◽  
Author(s):  
K Marthinsen ◽  
H Matsuhata ◽  
R Hfier ◽  
J Gjfnnes
Keyword(s):  
Electron Diffraction ◽  
Structure Factor ◽  
Bloch Wave ◽  
Critical Voltage ◽  
Dispersion Surface ◽  
Structure Factors ◽  
Three Phase ◽  
Convergent Beam ◽  
Diffraction Condition

The treatment of non-systematic multiple-beam effects in dynamical diffraction is extended. Expressions for Bloch wave degeneracies are given in the centrosymmetrical four-beam case and for some symmetrical directions. These degeneracies can be determined experimentally either as critical voltages or by locating the exact diffraction condition at a fixed voltage. The accuracy when applied to structure factor determination is comparable with the systematical critical voltage, namely 1% in UfT The three-beam case 0, g, h is treated as well in the non-centrosymmetrical case, where it can be used for determination of phases. It is shown that the contrast features can be represented .by an effective structure factor defined by the gap at the dispersion surface. From the variation in the gap with diffraction condition, a method to determine the three-phase structure invariant I\J = 9 + _ h + h _ 9 is given. The method is based upon the contrast asymmetry in the weaker diffracted beam and can be applied in Kikuchi, convergent beam or channelling patterns. Calculations relating to channelling in backscattering are also presented.

Sign in / Sign up

Export Citation Format

Share Document