Yi-Shan Huang

Quantitative phase determination for macromolecular crystals using stereoscopic multibeam imaging

Without invoking anomalous dispersion and heavy-atom derivatives, it is demonstrated that it is possible to directly determine the phases of a large number of reflections collected in a short time from macromolecular crystals using a stereoscopic oscillation-crystal imaging technique, in a multibeam diffraction geometry, where two crystallographic axes in opposite directions are employed as the rotation axes. The intensity profiles (distributions) of the diffraction spots versus the varying tilt Bragg angle of the rotation axis in the two stereoscopically related images yield quantitative phase information. Many multiple diffraction profiles of tetragonal lysozyme and an unknown protein structure are obtained at the rate of 100 profiles per 30 min of X-ray exposure.

The phenomenon of polarization suppression of X-ray Umweg multiple waves in crystals

The phenomenon of the polarization suppression of X-ray Umweg multiple waves in Renninger scans [Renninger (1937). Z. Kristallogr. 97, 107–121] of crystals, showing intensity decrease due to properly chosen wavelength and polarization of incident radiation, is observed. That is, one of the participating wave components in the multiple-wave interference is reduced considerably so that the intensity of multiple diffraction is decreased. The condition for total suppression of the multiple-wave interaction in crystals is derived theoretically from the Born approximation and verified with exact dynamical calculation and experiments. Partial suppression of the strong Umweg interfered component is demonstrated using elliptically or linearly polarized synchrotron radiation. The suppressed multiple-wave intensity distribution reveals high sensitivity to X-ray reflection phase. This multiple-diffraction technique under partial polarization suppression provides an alternative way of enhancing the visibility of multiple-wave interference in crystals for direct phase determination.

Polarization-resolved output analysis of X-ray multiple-wave interaction

The polarization suppression of the interfering components in X-ray multiple-wave interaction is observed for the first time by using a polarization analyzer with an arbitrary inclination of the diffraction plane with respect to that of the investigated crystal. The condition for total suppression of the multiple-wave interaction outside the investigated crystals by a polarization analyzer is derived theoretically from the modified Born approximation. By means of the partial suppression of the strong interfering component, the increase in the visibility of multiple-wave interference is experimentally and theoretically demonstrated. The proposed experimental polarization-resolved technique provides an operational way to enhance the visibility of X-ray multiple-wave interaction outside the investigated crystals for direct phase determination.

Quasi-universality and scaling behaviour of three-wave X-ray interference in crystals: A novel way for the quantitative determination of X-ray reflection phases

Abstract A quasi-universal function describing the intensity distribution of three-wave X-ray interaction in single crystals is derived for the first time from X-ray dynamical theory under the Bethe approximation for inversion-symmetry related reflections. The intensity distributions of three-wave interference can be scaled down to this dimensionless universal function with proper scaling factors. A newly derived intensity-ratio formula provides a new way of analyzing three-wave diffraction data for direct quantitative determination of X-ray reflection phases of complex systems involving macromolecules.

Anomalous Dispersion Behavior of Multiple-Wave X-Ray Diffraction at Absorption Edges

The effects of anomalous dispersion (resonance) on multiple reflection of x rays and their interference in crystals at atomic absorption edges are studied. Intensity ratios of two inversion-symmetry-related multiple diffractions at or near absorption edges exhibit highly phase-sensitive profiles with strong asymmetric characteristics, unlike those far from the edges. A new resonance perturbation Bethe approach is developed to explain this behavior. This leads to direct determination of the phase change for x-ray reflections at resonance.

X-Ray Diffraction Studies of the Recrystallization of C60-Based Polymers

Abstract A time-dependent x-ray scattering study is presented of the kinetics of the C60-based star polymer containing 6 urethane-connected polyether and the star model polymers containing 4, 3, and 2 urethane-connected polyether arms. By varying the temperature from 40°C to -40°C, the order-disorder phase transition (recrystallization) of the polymers has been observed. Two crystalline domains with the periodicities of 4.5±0.6 A and 3.7±0.4 A were detected. The domain sizes ranging from 70 A to 250 A, the transition temperatures from -15°C to 25°C and the maximum percentage of recrystallization from 13% to 34% increase as the number of polyether arms increases. The x-ray scattering peaks of the order phase grow up as I1 +I2(l - e−t/t0), where I1 and I2 are the initial intensity and the proportional intensity modulus, respectively. The relaxation time t0 of the order phase is varying as a power law with respect to the reduced temperature TR(=(T - TC)/TC): t0 = (35±10)·|TR|−1.42±0.07 seconds for the C60-ba...

Substrate-mediated multiwave resonance grazing incidence x-ray diffraction in thin films: A method for direct phase determination

Direct phase determination of surface in-plane reflection is realized for thin films on substrates by using substrate reflections as an intermediary to enhance the coherent interaction in resonant multiwave grazing incidence diffraction in thin films. The coupling of the in-plane diffracted waves at the interface between the thin film and the substrate is essential. The intensity variation due to this enhanced interaction/coupling becomes clearly visible, thus leading to unambiguous phase determination. This opens a different way for direct phase determination of surface reflections in thin films.

Polarization Suppression of X-rayUmwegMultiple Waves in Crystals

The phenomenon of the polarization suppression of X-ray Umweg multiple waves in Renninger scans [Renninger (1937). Z. Kristallogr. 97, 107-121] of crystals, showing intensity decrease due to properly chosen wavelength and polarization of incident radiation, is observed. That is, one of the participating wave components in the multiple-wave interference is reduced considerably so that the intensity of multiple diffraction is decreased. The condition for total suppression of the multiple-wave interaction in crystals is derived theoretically from the Born approximation and verified with exact dynamical calculation and experiments. Partial suppression of the strong Umweg interfered component is demonstrated using elliptically or linearly polarized synchrotron radiation. The suppressed multiple-wave intensity distribution reveals high sensitivity to X-ray reflection phase. This multiple-diffraction technique under partial polarization suppression provides an alternative way of enhancing the visibility of multiple-wave interference in crystals for direct phase determination.