scholarly journals Nitrosonium nitrate (NO+NO3 −) structure solution using in situ single-crystal X-ray diffraction in a diamond anvil cell

IUCrJ ◽  
2021 ◽  
Vol 8 (2) ◽  
pp. 208-214
Author(s):  
Dominique Laniel ◽  
Bjoern Winkler ◽  
Egor Koemets ◽  
Timofey Fedotenko ◽  
Stella Chariton ◽  
...  
Keyword(s):  
Single Crystal ◽  
Density Functional ◽  
High Pressures ◽  
Density Functional Theory Calculations ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molecular Systems ◽  
Structure Solution ◽  
Diamond Anvil

At high pressures, autoionization – along with polymerization and metallization – is one of the responses of simple molecular systems to a rise in electron density. Nitrosonium nitrate (NO+NO3 −), known for this property, has attracted a large interest in recent decades and was reported to be synthesized at high pressure and high temperature from a variety of nitrogen–oxygen precursors, such as N2O4, N2O and N2–O2 mixtures. However, its structure has not been determined unambiguously. Here, we present the first structure solution and refinement for nitrosonium nitrate on the basis of single-crystal X-ray diffraction at 7.0 and 37.0 GPa. The structure model (P21/m space group) contains the triple-bonded NO+ cation and the NO3 − sp 2-trigonal planar anion. Remarkably, crystal-chemical considerations and accompanying density-functional-theory calculations show that the oxygen atom of the NO+ unit is positively charged – a rare occurrence when in the presence of a less-electronegative element.

Investigation of Structural Evolution of Li1.1V3O8 by In Situ X-ray Diffraction and Density Functional Theory Calculations

2017 ◽  
Vol 29 (5) ◽  
pp. 2364-2373 ◽  
Author(s):  
Qing Zhang ◽  
Alexander B. Brady ◽  
Christopher J. Pelliccione ◽  
David C. Bock ◽  
Andrea M. Bruck ◽  
...  
Keyword(s):  
Density Functional Theory ◽  
Density Functional ◽  
Structural Evolution ◽  
Density Functional Theory Calculations ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray

High-quality structures at high pressure? Insights from inclusions in diamonds

2016 ◽  
Vol 231 (8) ◽  
Author(s):  
Ross J. Angel ◽  
Sula Milani ◽  
Matteo Alvaro ◽  
Fabrizio Nestola
Keyword(s):  
High Pressure ◽  
Single Crystal ◽  
High Pressures ◽  
Dominant Factor ◽  
Good Precision ◽  
Ambient Conditions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Experimental Protocols ◽  
Diamond Anvil

AbstractWe describe the experimental protocols necessary to measure the crystal structures of minerals trapped within diamonds by single-crystal X-ray diffraction to the same quality as obtained from minerals studied at ambient conditions. The results show that corrections for X-ray absorption in complex cases can be made with good precision. Comparison of the refined structure of a single-crystal olivine inclusion inside a diamond with the structure of a similar olivine held in a high-pressure diamond-anvil cell shows that data resolution, not the correction for absorption effects, is the dominant factor in influencing the quality of structures determined at high pressures by single-crystal X-ray diffraction.

scholarly journals Experimental Issues in In-Situ Synchrotron X-Ray Diffraction at High Pressure and Temperature by Using a Laser-Heated Diamond-Anvil Cell

1997 ◽  
Vol 499 ◽  
Author(s):  
C. S. Yoo ◽  
H. Cynn ◽  
A. Campbell ◽  
J.-Z. Hu
Keyword(s):  
Diamond Anvil Cell ◽  
High Pressures ◽  
Thermal Gradients ◽  
X Ray Diffraction ◽  
High Pressure And Temperature ◽  
X Ray ◽  
Diamond Anvil ◽  
Integrated Technique ◽  
Laser Heated

ABSTRACTAn integrated technique of diamond-anvil cell, laser-heating and synchrotron x-ray diffraction technologies is capable of structural investigation of condensed matter in an extended region of high pressures and temperatures above 100 GPa and 3000 K. The feasibility of this technique to obtain reliable data, however, strongly depends on several experimental issues, including optical and x-ray setups, thermal gradients, pressure homogeneity, preferred orientation, and chemical reaction. In this paper, we discuss about these experimental issues together with future perspectives of this technique for obtaining accurate data.

Single-crystal X-ray diffraction at high pressures with diamond-anvil cells

1992 ◽  
Vol 39 (1-4) ◽  
pp. 13-32 ◽  
Author(s):  
R. J. Angel ◽  
N. L. Ross ◽  
I. G. Wood ◽  
P. A. Woods
Keyword(s):  
Single Crystal ◽  
High Pressures ◽  
X Ray Diffraction ◽  
Diamond Anvil Cells ◽  
X Ray ◽  
Diamond Anvil

scholarly journals Ba3CrN3H: A New Nitride-Hydride with Trigonal Planar Cr4+

2018 ◽  
Author(s):  
Nathaniel W. Falb ◽  
Jennifer N. Neu ◽  
Tiglet Besara ◽  
Jeffrey B. Whalen ◽  
David J. Singh ◽  
...  
Keyword(s):  
Density Functional Theory ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Single Crystal ◽  
Density Functional ◽  
Density Functional Theory Calculations ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray ◽  
Crystal Synthesis

Single crystal synthesis of a new nitride-hydride Ba3CrN3H. X-ray diffraction, nuclear magnetic resonance, and bond-valance sum and density functional theory calculations confirmed the presence and location of the anionic hydrogen in this compound.

scholarly journals Synthesis of dinucleoside acylphosphonites by phosphonodiamidite chemistry and investigation of phosphorus epimerization

2015 ◽  
Vol 11 ◽  
pp. 184-191 ◽  
Author(s):  
William H Hersh
Keyword(s):  
Density Functional Theory ◽  
Single Crystal ◽  
Density Functional ◽  
Density Functional Theory Calculations ◽  
X Ray Diffraction ◽  
Inversion Barrier ◽  
Functional Theory ◽  
Acyl Chlorides ◽  
X Ray

The reaction of the diamidite, (iPr2N)2PH, with acyl chlorides proceeds with the loss of HCl to give the corresponding acyl diamidites, RC(O)P(N(iPr)2)2 (R = Me (7), Ph (9)), without the intervention of sodium to give a phosphorus anion. The structure of 9 was confirmed by single-crystal X-ray diffraction. The coupling of the diamidites 7 and 9 with 5′-O-DMTr-thymidine was carried out with N-methylimidazolium triflate as the activator to give the monoamidites 3′-O-(P(N(iPr)2)C(O)R)-5′-O-DMTr-thymidine, and further coupling with 3′-O-(tert-butyldimethylsilyl)thymidine was carried out with activation by pyridinium trifluoroacetate/N-methylimidazole. The new dinucleoside acylphosphonites could be further oxidized, hydrolyzed to the H-phosphonates, and sulfurized to give the known mixture of diastereomeric phosphorothioates. The goal of this work was the measurement of the barrier to inversion of the acylphosphonites, which was expected to be low by analogy to the low barrier found in acylphosphines. However, the barrier was found to be high as no epimerization was detected up to 150 °C, and consistent with this, density functional theory calculations give an inversion barrier of over 40 kcal/mol.

Anisotropic thermal expansion of calcite at high pressures; an in situ X-ray diffraction study in a hydrothermal diamond-anvil cell

1995 ◽  
Vol 80 (9-10) ◽  
pp. 941-946 ◽  
Author(s):  
Tzy-Chung Wu ◽  
Andy H. Shen ◽  
Maura S. Weathers ◽  
William A. Bassett ◽  
I-Ming Chou
Keyword(s):  
Thermal Expansion ◽  
Diffraction Study ◽  
Diamond Anvil Cell ◽  
High Pressures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anisotropic Thermal Expansion ◽  
Diamond Anvil

scholarly journals Compression behavior of Sm2Ti2O7-pyrochlore up to 50 GPa: single-crystal X-ray diffraction and density functional theory calculations

2014 ◽  
Vol 59 (36) ◽  
pp. 5278-5282 ◽  
Author(s):  
Björn Winkler ◽  
Alexandra Friedrich ◽  
Wolfgang Morgenroth ◽  
Eiken Haussühl ◽  
Victor Milman ◽  
...  
Keyword(s):  
Density Functional Theory ◽  
Single Crystal ◽  
Density Functional ◽  
Density Functional Theory Calculations ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
Compression Behavior ◽  
X Ray

scholarly journals Single-crystal diffraction at the high-pressure Indo-Italian beamline Xpress at Elettra, Trieste

2020 ◽  
Vol 27 (1) ◽  
pp. 222-229 ◽  
Author(s):  
Paolo Lotti ◽  
Sula Milani ◽  
Marco Merlini ◽  
Boby Joseph ◽  
Frederico Alabarse ◽  
...  
Keyword(s):  
High Pressure ◽  
Single Crystal ◽  
Structural Features ◽  
Atomic Scale ◽  
Experimental Setup ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diamond Anvil ◽  
Synthetic Crystal

In this study the first in situ high-pressure single-crystal X-ray diffraction experiments at Xpress, the Indo-Italian beamline of the Elettra synchrotron, Trieste (Italy), are reported. A description of the beamline experimental setup and of the procedures for single-crystal centring, data collection and processing, using diamond anvil cells, are provided. High-pressure experiments on a synthetic crystal of clinoenstatite (MgSiO3), CaCO3 polymorphs and a natural sample of leucophoenicite [Mn7Si3O12(OH)2] validated the suitability of the beamline experimental setup to: (i) locate and characterize pressure-induced phase transitions; (ii) solve ab initio the crystal structure of high-pressure polymorphs; (iii) perform fine structural analyses at the atomic scale as a function of pressure; (iv) disclose complex symmetry and structural features undetected using conventional X-ray sources.

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