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High Pressure Single Crystal Diffraction at PX^2
In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the GSECARS 13-BM-C beamline at the Advanced Photon Source. The DAC program at 13-BM-C is part of the Partnership for Extreme Xtallography (PX^2) project. B...
Autores principales: | , , , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
MyJove Corporation
2017
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5352262/ https://www.ncbi.nlm.nih.gov/pubmed/28117811 http://dx.doi.org/10.3791/54660 |
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author | Zhang, Dongzhou Dera, Przemyslaw K. Eng, Peter J. Stubbs, Joanne E. Zhang, Jin S. Prakapenka, Vitali B. Rivers, Mark L. |
author_facet | Zhang, Dongzhou Dera, Przemyslaw K. Eng, Peter J. Stubbs, Joanne E. Zhang, Jin S. Prakapenka, Vitali B. Rivers, Mark L. |
author_sort | Zhang, Dongzhou |
collection | PubMed |
description | In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the GSECARS 13-BM-C beamline at the Advanced Photon Source. The DAC program at 13-BM-C is part of the Partnership for Extreme Xtallography (PX^2) project. BX-90 type DACs with conical-type diamond anvils and backing plates are recommended for these experiments. The sample chamber should be loaded with noble gas to maintain a hydrostatic pressure environment. The sample is aligned to the rotation center of the diffraction goniometer. The MARCCD area detector is calibrated with a powder diffraction pattern from LaB(6). The sample diffraction peaks are analyzed with the ATREX software program, and are then indexed with the RSV software program. RSV is used to refine the UB matrix of the single crystal, and with this information and the peak prediction function, more diffraction peaks can be located. Representative single crystal diffraction data from an omphacite (Ca(0.51)Na(0.48))(Mg(0.44)Al(0.44)Fe(2+)(0.14)Fe(3+)(0.02))Si(2)O(6) sample were collected. Analysis of the data gave a monoclinic lattice with P2/n space group at 0.35 GPa, and the lattice parameters were found to be: a = 9.496 ±0.006 Å, b = 8.761 ±0.004 Å, c = 5.248 ±0.001 Å, β = 105.06 ±0.03º, α = γ = 90º. |
format | Online Article Text |
id | pubmed-5352262 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2017 |
publisher | MyJove Corporation |
record_format | MEDLINE/PubMed |
spelling | pubmed-53522622017-04-04 High Pressure Single Crystal Diffraction at PX^2 Zhang, Dongzhou Dera, Przemyslaw K. Eng, Peter J. Stubbs, Joanne E. Zhang, Jin S. Prakapenka, Vitali B. Rivers, Mark L. J Vis Exp Chemistry In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the GSECARS 13-BM-C beamline at the Advanced Photon Source. The DAC program at 13-BM-C is part of the Partnership for Extreme Xtallography (PX^2) project. BX-90 type DACs with conical-type diamond anvils and backing plates are recommended for these experiments. The sample chamber should be loaded with noble gas to maintain a hydrostatic pressure environment. The sample is aligned to the rotation center of the diffraction goniometer. The MARCCD area detector is calibrated with a powder diffraction pattern from LaB(6). The sample diffraction peaks are analyzed with the ATREX software program, and are then indexed with the RSV software program. RSV is used to refine the UB matrix of the single crystal, and with this information and the peak prediction function, more diffraction peaks can be located. Representative single crystal diffraction data from an omphacite (Ca(0.51)Na(0.48))(Mg(0.44)Al(0.44)Fe(2+)(0.14)Fe(3+)(0.02))Si(2)O(6) sample were collected. Analysis of the data gave a monoclinic lattice with P2/n space group at 0.35 GPa, and the lattice parameters were found to be: a = 9.496 ±0.006 Å, b = 8.761 ±0.004 Å, c = 5.248 ±0.001 Å, β = 105.06 ±0.03º, α = γ = 90º. MyJove Corporation 2017-01-16 /pmc/articles/PMC5352262/ /pubmed/28117811 http://dx.doi.org/10.3791/54660 Text en Copyright © 2017, Journal of Visualized Experiments http://creativecommons.org/licenses/by-nc-nd/3.0/ This is an open-access article distributed under the terms of the Creative Commons Attribution-NonCommercial-NoDerivs 3.0 Unported License. To view a copy of this license, visithttp://creativecommons.org/licenses/by-nc-nd/3.0/ |
spellingShingle | Chemistry 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 PX^2 |
title | High Pressure Single Crystal Diffraction at PX^2 |
title_full | High Pressure Single Crystal Diffraction at PX^2 |
title_fullStr | High Pressure Single Crystal Diffraction at PX^2 |
title_full_unstemmed | High Pressure Single Crystal Diffraction at PX^2 |
title_short | High Pressure Single Crystal Diffraction at PX^2 |
title_sort | high pressure single crystal diffraction at px^2 |
topic | Chemistry |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5352262/ https://www.ncbi.nlm.nih.gov/pubmed/28117811 http://dx.doi.org/10.3791/54660 |
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