Structural insights intoM2O–Al2O3–WO3(M= Na, K) system by electron diffraction tomography

Andrusenko, Iryna; Krysiak, Yaşar; Mugnaioli, Enrico; Gorelik, Tatiana E.; Nihtianova, D.; Kolb, Ute

doi:10.1107/s2052520615007994

Cited by 6 publications

(4 citation statements)

References 57 publications

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“…Although in the past few years precession electron diffraction tomography (PEDT) has allowed the solution of many complex nanostructures of catalysts, , metal–organic hybrids, , minerals, , intermetallics, , and other kinds of inorganic compounds, , there are still a very limited number of examples concerning organic compounds. , This is mainly due to the high beam sensitivity of these materials and the general need to use TEM cryocooling techniques to slow down the radiation damage. , …”

Section: Introductionmentioning

confidence: 99%

Crystal Structures of Two Important Pharmaceuticals Solved by 3D Precession Electron Diffraction Tomography

Das¹,

Mugnaioli

Nicolopoulos³

et al. 2018

Org. Process Res. Dev.

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The crystal structures of two important marketed pharmaceuticals, namely, ramelteon (RAM) and tolvaptan (TOL), were determined for the first time using 3D precession electron diffraction tomography (PEDT) on 500 nm-sized crystals. The results were compared with the same structures determined by single-crystal X-ray diffraction on subsequently grown 50−200 μm single crystals, indicating a good match of molecular conformation, crystal packing, and unit cell parameters. The X-ray crystal structures were used to validate the developed workflow of data acquisition and structure solution with electron diffraction. This study highlights that 3D PEDT alone is able to provide accurate crystal structures from pharmaceutical nanocrystals that will suffice for most practical applications when no larger crystals can be grown.

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Section: Introductionmentioning

confidence: 99%

Crystal Structures of Two Important Pharmaceuticals Solved by 3D Precession Electron Diffraction Tomography

Das¹,

Mugnaioli

Nicolopoulos³

et al. 2018

Org. Process Res. Dev.

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“…Some of its members behave as promising laser host materials for transition metal and lanthanide ions due to their high and continuous transparency in the wide range of the near-IR region. For instance, Cr 3+ -doped KAl(MoO 4 ) 2 crystal has been proven to be a suitable laser host, characterized by high absorption, efficient pumping, and broad laser emission [7]. As a member of M I M III (M VI O 4 ) 2 , KAl(MoO 4 ) 2 represents the large crystal family with layered structure.…”

Section: Introductionmentioning

confidence: 99%

In-Situ Studies of Structure Transformation and Al Coordination of KAl(MoO4)2 during Heating by High Temperature Raman and 27Al NMR Spectroscopies

et al. 2017

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Recent interest in optimizing composition and synthesis conditions of functional crystals, and the further exploration of new possible candidates for tunable solid-state lasers, has led to significant research on compounds in this family MIMIII(MVIO4)2 (MI = alkali metal, MIII = Al, In, Sc, Fe, Bi, lanthanide; MVI = Mo, W). The vibrational modes, structure transformation, and Al coordination of crystalline, glassy, and molten states of KAl(MoO4)2 have been investigated by in-situ high temperature Raman scattering and 27Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy, together with first principles density functional simulation of room temperature Raman spectrum. The results showed that, under the present fast quenching conditions, Al is present predominantly in [AlO6] octahedra in both KAl(MoO4)2 glass and melt, with the tetrahedrally coordinated Al being minor at approximately 2.7%. The effect of K+, from ordered arrangement in the crystal to random distribution in the melt, on the local chemical environment of Al, was also revealed. The distribution and quantitative analysis of different Al coordination subspecies are final discussed and found to be dependent on the thermal history of the glass samples.

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“…Even if part of the structure is significantly altered during data collection, the large amount of collected intensities should allow recognizing the true Laue group. Systematic extinctions (especially zonal ones) could also be determined unambiguously, further restricting the space group choice (Camalli et al, 2012;Andrusenko et al, 2015). Especially prone to vacuum-induced dehydration J.…”

Section: Introductionmentioning

confidence: 99%

Structural study of decrespignyite-(Y), a complex yttrium rare earth copper carbonate chloride, by three-dimensional electron and synchrotron powder diffraction

et al. 2020

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Abstract. The crystal structure of the mineral decrespignyite-(Y) from the Paratoo copper mine (South Australia) has been obtained by applying δ recycling direct methods to 3D electron diffraction (ED) data followed by Rietveld refinements of synchrotron data. The unit cell is a= 8.5462(2), c= 22.731(2) Å and V= 1437.8(2) Å3, and the chemical formula for Z=1 is (Y10.35REE1.43Ca0.52Cu5.31)Σ17.61(CO3)14Cl2.21(OH)16.79⋅18.35H2O (REE: rare earth elements). The ED data are compatible with the trigonal P3‾m1 space group (no. 164) used for the structure solution (due to the disorder affecting part of the structure, the possibility of a monoclinic unit cell cannot completely be ruled out). The structure shows metal layers perpendicular to [001], with six independent positions for Y, REE and Cu (sites M1 to M4 are full, and sites M5 and M6 are partially vacant), and two other sites, Cu1 and Cu2, partially occupied by Cu. One characteristic of decrespignyite is the existence of hexanuclear (octahedral) oxo-hydroxo yttrium clusters [Y6(μ6-O)(μ3-OH)8O24] (site M1) with the 24 bridging O atoms belonging to two sets of symmetry-independent (CO3)2− ions, with the first set (2×) along a ternary axis giving rise to a layer of hexanuclear clusters and the second set (6×) tilted and connecting the hexanuclear clusters with hetero-tetranuclear ones hosting Cu, Y and REE (M2 and M3 sites). The rest of the crystal structure consists of two consecutive M3 + M4 layers containing the partially occupied M5, M6, and Cu2 sites and additional carbonate anions in between. The resulting structure model is compatible with the chemical analysis of the type material which is poorer in Cu and richer in (REE, Y) than the above-described material.

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Structural insights intoM₂O–Al₂O₃–WO₃(M= Na, K) system by electron diffraction tomography

Cited by 6 publications

References 57 publications

Crystal Structures of Two Important Pharmaceuticals Solved by 3D Precession Electron Diffraction Tomography

Crystal Structures of Two Important Pharmaceuticals Solved by 3D Precession Electron Diffraction Tomography

In-Situ Studies of Structure Transformation and Al Coordination of KAl(MoO4)2 during Heating by High Temperature Raman and 27Al NMR Spectroscopies

Structural study of decrespignyite-(Y), a complex yttrium rare earth copper carbonate chloride, by three-dimensional electron and synchrotron powder diffraction

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