Single Crystal X-Ray Structure Analysis under High Pressure Using He Gas as a Pressure Transmitting Medium. Crystal Structure of Mixed-Valence Complexes Cs2AuIAuIIIX6.

Abstract Opaque blue crystals of a new mixed valence cerium germanate have been prepared at elevated temperatures (1555 K) under careful thermoanalytical control. Single crystal structure analysis shows three different types of germanate anions [GeO4]4-, [Ge2O7]6- and [Ge3O10]8-, all germanium atoms being in tetrahedral coordination. Due to the larger number of oxygens per unit cell (Ce2Ge2O7.2), with all the oxygens unambiguously located by X-ray single crystal structure analysis, this phase differs significantly from the corresponding cerium(III) germanate Ce2Ge2O7, which shows [GeO4]4- and [Ge3O10]8-, but no [Ge2O7]6- ditetrahedral groupings.

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Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

10.26434/chemrxiv.11345063.v2 ◽

2020 ◽

Author(s):

Keishiro Yamashita ◽

Kazuki Komatsu ◽

Hiroyuki Kagi

Keyword(s):

Crystal Structure ◽

High Pressure ◽

Crystal Growth ◽

Single Crystal ◽

Room Temperature ◽

Growth Technique ◽

Salt Hydrate ◽

X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

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Crystal Structure Analysis of the First Discovered Stability-Enhanced Solid State of Tenofovir Disoproxil Free Base Using Single Crystal X-ray Diffraction

Molecules ◽

10.3390/molecules22071182 ◽

2017 ◽

Vol 22 (7) ◽

pp. 1182 ◽

Cited By ~ 2

Author(s):

Ji-Hun An ◽

Alice Kiyonga ◽

Woojin Yoon ◽

Hyung Ryu ◽

Jae-Sun Kim ◽

...

Keyword(s):

Crystal Structure ◽

Solid State ◽

Single Crystal ◽

Structure Analysis ◽

Crystal Structure Analysis ◽

Free Base ◽

X Ray Diffraction ◽

X Ray

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Single crystal structure analysis of the Se-incorporated mordenite, coupled with the anomalous X-ray scattering

Solid State Sciences ◽

10.1016/j.solidstatesciences.2010.10.018 ◽

2011 ◽

Vol 13 (4) ◽

pp. 684-690 ◽

Cited By ~ 5

Author(s):

N. Togashi ◽

K. Sugiyama ◽

J. Yu ◽

S. Qiu ◽

O. Terasaki

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Structure Analysis ◽

Crystal Structure Analysis ◽

Single Crystal Structure ◽

X Ray ◽

X Ray Scattering ◽

Single Crystal Structure Analysis ◽

Ray Scattering

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Syntheses and Characterization of N,N'-Dipropyl-1,2-ethanediamine and N,N'-diisopropyl-1,2-ethanediamine Complexes of Nickel(II): Thermal Studies and X-Ray Single Crystal Structure Analysis of [Ni(N,N'-Dipropyl-1,2-ethanediamine)2(NCS)2].

Acta Chemica Scandinavica ◽

10.3891/acta.chem.scand.52-0702 ◽

1998 ◽

Vol 52 ◽

pp. 702-708 ◽

Cited By ~ 4

Author(s):

Inamur Rahaman Laskar ◽

Debasis Das ◽

Golam Mostafa ◽

Alan J. Welch ◽

Nirmalendu Ray Chaudhuri ◽

...

Keyword(s):

Crystal Structure ◽

Single Crystal ◽

Structure Analysis ◽

Thermal Studies ◽

Crystal Structure Analysis ◽

Single Crystal Structure ◽

X Ray ◽

Single Crystal Structure Analysis

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Crystal Structures of Al2Cu Revisited: Understanding Existing Phases and Exploring Other Potential Phases

Metals ◽

10.3390/met9101037 ◽

2019 ◽

Vol 9 (10) ◽

pp. 1037 ◽

Cited By ~ 4

Author(s):

Sai Wang ◽

Changzeng Fan

Keyword(s):

Crystal Structure ◽

High Pressure ◽

Single Crystal ◽

First Principles ◽

First Principles Calculations ◽

X Ray Diffraction ◽

X Ray ◽

Structural Relationships ◽

Al2cu Phase ◽

High Pressure Sintering

When processing single crystal X-ray diffraction datasets for twins of Al2Cu sample synthesized by the high-pressure sintering (HPS) method, we have clarified why the crystal structure of Al2Cu was incorrectly solved about a century ago. The structural relationships between all existing Al2Cu phases, including the Owen-, θ-, θ’-, and Ω-Al2Cu phases, were investigated and established based on a proposed pseudo Al2Cu phase. Two potential phases have been built up by adjusting the packing sequences of A/B layers of Al atoms that were inherent in all existing Al2Cu phases. The mechanical, thermal, and dynamical stability of two such novel phases and their electronic properties were investigated by first-principles calculations.

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Microporous crystal structure of labuntsovite-Fe and high-pressure behavior up to 23 GPa

Acta Crystallographica Section B Structural Science Crystal Engineering and Materials ◽

10.1107/s205252061700498x ◽

2018 ◽

Vol 74 (1) ◽

pp. 1-11 ◽

Cited By ~ 1

Author(s):

Sergey M. Aksenov ◽

Elena A. Bykova ◽

Ramiza K. Rastsvetaeva ◽

Nikita V. Chukanov ◽

Irina P. Makarova ◽

...

Keyword(s):

Crystal Structure ◽

High Pressure ◽

Single Crystal ◽

Cross Section ◽

Structure Refinement ◽

Alkaline Complex ◽

X Ray ◽

Cell Parameters ◽

Diamond Anvil ◽

The Stability

Labuntsovite-Fe, an Fe-dominant member of the labuntsovite subgroup, was first discovered in the Khibiny alkaline massif on Mt Kukisvumchorr [Khomyakov et al. (2001). Zap. Vseross. Mineral. Oba, 130, 36–45]. However, no data are published about the crystal structure of this mineral. Labuntsovite-Fe from a peralkaline pegmatite located on Mt Nyorkpakhk, in the Khibiny alkaline complex, Kola Peninsula, Russia, has been investigated by means of electron microprobe analyses, single-crystal X-ray structure refinement, and IR and Raman spectroscopies. Monoclinic unit-cell parameters of labuntsovite-Fe are: a = 14.2584 (4), b = 13.7541 (6), c = 7.7770 (2) Å, β = 116.893 (3)°; V = 1360.22 (9) Å3; space group C2/m. The structure was refined to final R 1 = 0.0467, wR 2 = 0.0715 for 3202 reflections [I > 3σ(I)]. The refined crystal chemical formula is (Z = 2): Na2K2Ba0.7[(Fe0.5Ti0.1Mg0.05)(H2O)1.3]{[Ti2(Ti1.9Nb0.1)(O,OH)4][Si4O12]2}·4H2O. The high-pressure in situ single-crystal X-ray diffraction study of the labuntsovite-Fe has been carried out in a diamond anvil cell. The labuntsovite-type structure is stable up to 23 GPa and phase transitions are not observed. Calculations using the BM3 equation of state resulted in the bulk modulus K = 72 (2) GPa, K′0 = 3.7 (2) and V 0 = 1363 (2) Å3. Compressing of the heteropolyhedral zeolite-like framework leads to the deformation of main structural units. Octahedral rods show the gradual increase of distortion and the wave-like character of rods becomes more distinct. Rod deformations result in the distortion of the silicon–oxygen ring which is not equal in different directions. Structural channels are characterized by a different ellipticity–pressure relationship: the cross-section of the largest channel I and channel II demonstrates the stability of the geometrical characteristics which practically do not depend on pressure: ∊channel I ≃ 0.85 (4) (cross-section is rather regular) and ∊channel II ≃ 0.52 (2) within the whole pressure range. However, channel III is characterized by the increasing of ellipticity with pressure (∊ = 0.40 → 0.10).

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