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Title: High Pressure Single Crystal Diffraction at PX 2

Abstract

In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.

Authors:
; ; ; ; ; ;
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Org.:
USDOE; National Science Foundation (NSF)
OSTI Identifier:
1342241
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Visualized Experiments; Journal Volume: 119; Journal Issue: 119
Country of Publication:
United States
Language:
ENGLISH
Subject:
73 NUCLEAR PHYSICS AND RADIATION PHYSICS

Citation Formats

Zhang, Dongzhou, Dera, Przemyslaw K., Eng, Peter J., Stubbs, Joanne E., Zhang, Jin S., Prakapenka, Vitali B., and Rivers, Mark L. High Pressure Single Crystal Diffraction at PX2. United States: N. p., 2017. Web. doi:10.3791/54660.
Zhang, Dongzhou, Dera, Przemyslaw K., Eng, Peter J., Stubbs, Joanne E., Zhang, Jin S., Prakapenka, Vitali B., & Rivers, Mark L. High Pressure Single Crystal Diffraction at PX2. United States. doi:10.3791/54660.
Zhang, Dongzhou, Dera, Przemyslaw K., Eng, Peter J., Stubbs, Joanne E., Zhang, Jin S., Prakapenka, Vitali B., and Rivers, Mark L. Sun . "High Pressure Single Crystal Diffraction at PX2". United States. doi:10.3791/54660.
@article{osti_1342241,
title = {High Pressure Single Crystal Diffraction at PX2},
author = {Zhang, Dongzhou and Dera, Przemyslaw K. and Eng, Peter J. and Stubbs, Joanne E. and Zhang, Jin S. and Prakapenka, Vitali B. and Rivers, Mark L.},
abstractNote = {In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.},
doi = {10.3791/54660},
journal = {Journal of Visualized Experiments},
number = 119,
volume = 119,
place = {United States},
year = {Sun Jan 01 00:00:00 EST 2017},
month = {Sun Jan 01 00:00:00 EST 2017}
}
  • We performed the single-crystal X-ray diffraction study of a perovskite-type gold mixed-valence compound, Cs{sub 2}Au{sup I}Au{sup III}Cl{sub 6}, under high pressures up to 18 GPa by using a diamond-anvil-cell with helium gas as an ideal hydrostatic pressure-transmitting medium. The lattice parameters and the variable atomic positional parameters were obtained with reasonable accuracy at various pressures. A structural phase transition at ca. 12.5 GPa from I4/mmm to Pm3m was found. The lattice parameters a {sub 0} and c {sub 0}, denoted in the tetragonal cell setting, result in the relationship 2{sup 1/2} a {sub 0}=c {sub 0}, and the superstructure reflectionsmore » h k l (l is odd), caused by the shift of the Cl ions from the midpoint of the Au ions, disappeared at pressures above the phase transition. Both elongated [Au{sup III}Cl{sub 6}] and compressed [Au{sup I}Cl{sub 6}] octahedra in the low-pressure phase smoothly approach regular octahedra with increasing pressure. Above the structural phase transition at 12.5 GPa, all the [AuCl{sub 6}] octahedra are crystallographically equivalent, which shows that the tetragonal-to-cubic phase transition accompanies the valence transition from the Au{sup I}/Au{sup III} mixed-valence state to the Au{sup II} single-valence state. - Graphical abstract: Single-crystal X-ray diffraction study under high pressures up to 18 GPa by using a diamond-anvil-cell with helium gas as an ideal hydrostatic pressure medium has revealed that a perovskite-type gold mixed-valence compound, Cs{sub 2}Au{sup I}Au{sup III}Cl{sub 6}, exhibits the structural phase transition from tetragonal to cubic at 12.5 GPa accompanying gold valence transition.« less
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