Synthesis, revised crystal structures, and refractive indices of ABW-type CsMTiO4 (M = Al, Fe, Ga) and ANA-type CsTi1.10Si1.90O6.50, and the determination of the electronic polarizability of 4-coordinated Ti4+

2020 ◽  
Vol 235 (11) ◽  
pp. 533-551
Author(s):  
Jan Derk Groeneveld ◽  
Manfred Burianek ◽  
Johannes Birkenstock ◽  
Lennart A. Fischer ◽  
Robert D. Shannon ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Analyses ◽  
Charge Compensation ◽  
Refractive Indices ◽  
Electronic Polarizability ◽  
X Ray Diffraction ◽  
Wyckoff Position ◽  
The Difference ◽  
Diffraction Patterns

AbstractSingle crystals of ABW-type CsAlTiO4 (CAT), CsFeTiO4 (CFT), CsGaTiO4 (CGT), and ANA-type CsTi1.1Si1.9O6.5 (CST) were grown and characterized by electron microprobe analyses, single-crystal X-ray diffraction, thermal analyses, and spindle-stage optical investigations to determine the electronic polarizability of 4-coordinated Ti4+, α([4]Ti4+). The crystal structure of CAT was confirmed to crystallize in the highest possible topological symmetry Imma (a = 8.9677(2) Å, b = 5.7322(1) Å, c = 9.9612(3) Å) with tetrahedrally coordinated Al and Ti equally distributed on Wyckoff position 8i. Twinning by reticular merohedry with a twin index of 2 was observed for most of the crystals resulting in a hexagonal twin lattice (a = 11.487(3) Å, c = 8.968(2) Å) with Laue symmetry 6/mmm. Refractive indices measured by immersion methods on an untwinned specimen are nx = 1.716(5), ny = 1.725(2), and nz = 1.727(1) with 2Vz = 127.1(6)°. The diffraction patterns of CFT and CGT clearly showed superstructure reflections causing a symmetry lowering of index 4 with a transformation according to 2a, b, c from Imma to Pmab with a = 18.3054(7) Å, b = 5.8083(2) Å, c = 9.9938(4) Å for CFT, and a = 18.2921(6) Å, b = 5.7636(2) Å, c = 9.9210(3) Å for CGT. Refractive indices for CGT are nx = 1.750(3), ny = 1.772(3), and nz = 1.776(2) with 2Vz = 132(1)°. The crystal structure of the ANA-type CsTi1.1Si1.9O6.5 was confirmed to crystallize in space group Ia$\overline{3}$d (a = 13.8333(4) Å). The extra 0.5 O atoms are needed for charge compensation and to allow the sum of electronic polarizabilities to give a total electronic polarizability calculated from the refractive index n = 1.718(4). The electronic polarizability of [4]Ti4+ was calculated from the difference between the observed total polarizabilities (derived from the mean refractive indices of CAT and CGT) and the sum of electronic polarizabilities of cations and anions omitting the polarizability of Ti resulting in α([4]Ti4+) = 5.15(5) Å3.

scholarly journals Determination of the H<sub>2</sub>O content in minerals, especially zeolites, from their refractive indices based on mean electronic polarizabilities of cations

2020 ◽  
Vol 32 (1) ◽  
pp. 27-40
Author(s):  
Reinhard X. Fischer ◽  
Manfred Burianek ◽  
Robert D. Shannon
Keyword(s):  
Thermal Analyses ◽  
Refractive Indices ◽  
Formula Unit ◽  
Electronic Polarizability ◽  
Hydrous Minerals ◽  
A Value ◽  
Small Crystals ◽  
Zeolite Type ◽  
The Difference

Abstract. It is shown here that the H2O content of hydrous minerals can be determined from their mean refractive indices with high accuracy. This is especially important when only small single crystals are available. Such small crystals are generally not suitable for thermal analyses or for other reliable methods of measuring the amount of H2O. In order to determine the contribution of the H2O molecules to the optical properties, the total electronic polarizability is calculated from the anhydrous part of the chemical composition using the additivity rule for individual electronic polarizabilities of cations and anions. This anhydrous contribution is then compared with the total observed electronic polarizability calculated from the mean refractive index of the hydrous compound using the Anderson–Eggleton relationship. The difference between the two values represents the contribution of H2O. The amount can be derived by solving the equation αcalc=∑iniαicat+∑jαjo×10-NjVm1.2×nj+nW1.2+nw×αW for the number nw of H2O molecules per formula unit (pfu), with the electronic polarizabilities αcat for cations, the values N and αo describing the anion polarizabilities, the number n of cations and anions, and the molar volume Vm, using a value of αW=1.62 Å3 for the electronic polarizability of H2O. The equation is solved numerically, yielding the number nw of H2O molecules per formula unit. The results are compared with the observed H2O content evaluating 157 zeolite-type compounds and 770 non-zeolitic hydrous compounds, showing good agreement. This agreement is expressed by a factor relating the calculated to the observed numbers being close to 1 for the majority of compounds. Zeolites with occluded anionic or neutral species (SO3, SO4, CO2, or CO3) show unusually high deviations between the calculated and observed amount of H2O, indicating that the polarizabilities of these species should be treated differently in zeolites and zeolite-type compounds.

scholarly journals Crystal structure of the thortveitite-relatedMphase, (MnxZn1–x)2V2O7(0.75

2018 ◽  
Vol 74 (10) ◽  
pp. 1079-1087
Author(s):  
Kevin M. Knowles ◽  
Anjan Sil ◽  
Berthold Stöger ◽  
Matthias Weil
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Distorted Version ◽  
Triclinic Structure ◽  
Diffraction Patterns ◽  
Triclinic Unit Cell

The determination of the crystal structure of theMphase, (MnxZn1–x)2V2O7(0.75 <x< 0.913), in the pseudobinary Mn2V2O7–Zn2V2O7system forx≃ 0.8 shows that the previously published triclinic unit-cell parameters for this thortveitite-related phase do not describe a true lattice for this phase. Instead, single-crystal X-ray data and Rietveld refinement of synchrotron X-ray powder data show that theMphase has a different triclinic structure in the space groupP-1 withZ= 2. As prior work has suggested, the crystal structure can be described as a distorted version of the thortveitite crystal structure of β-Mn2V2O7. A twofold superstructure in diffraction patterns of crystals of theMphase used for single-crystal X-ray diffraction work arises from twinning by reticular pseudomerohedry. This superstructure can be described as a commensurate modulation of a pseudo-monoclinic basis structure closely related to the crystal structure of β-Mn2V2O7. In comparison with the distortions introduced when β-Mn2V2O7transforms at low temperature to α-Mn2V2O7, the distortions which give rise to theMphase from the β-Mn2V2O7prototype are noticeably less pronounced.

THE HYDRATION OF THE ALUMINATES OF CALCIUM.: II. THE HYDRATION PRODUCTS OF TRICALCIUM ALUMINATE

1929 ◽  
Vol 1 (3) ◽  
pp. 201-213 ◽  
Author(s):  
T. Thorvaldson ◽  
N. S. Grace ◽  
V. A. Vigfusson
Keyword(s):  
Crystal Structure ◽  
Refractive Indices ◽  
Vapor Pressures ◽  
Hydration Products ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hexagonal Form ◽  
Tricalcium Aluminate ◽  
Diffraction Patterns ◽  
Crystalline Forms

Further studies on the isometric form of hydrated tricalcium aluminate are reported. These include methods of preparation, crystalline forms, X-ray diffraction pattern, and determinations of solubility and density. The products formed when the hexagonal form of hydrated tricalcium aluminate is dehydrated at definite vapor pressures of Water at 21 °C., were studied. The density, refractive indices, heats of solution in HCl.200 H2O, and the X-ray diffraction patterns of several probable hydrates were determined. The experimental evidence given indicates that hydrates of 3CaO.Al2O3 having 6, 8, 91/2, 101/2, and 12 moles of water are formed, but that the water in excess of 8 moles is very loosely held and that its removal does not materially affect the crystal structure. The exact composition of some of the higher hydrates requires confirmation.

scholarly journals Indexing the Diffraction Patterns and Investigating the Crystal Structure of Pb-doped Strontium Ferrites

2013 ◽  
Vol 5 (2) ◽  
pp. 235-244 ◽  
Author(s):  
Z. Ullah ◽  
S. Atiq ◽  
S. Naseem
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Hexagonal Phase ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Auto Ignition ◽  
Ray Density ◽  
Diffraction Patterns

Strontium hexaferrites were prepared in powder form by sol-gel auto-ignition technique and Pb was doped in different concentrations to attain the various compositions Sr1-xPbxFe12O19 (x = 0.00, 0.05, 0.10, 0.15, 0.20). Sintering treatment of the samples was made at 800 oC for the development of stable hexagonal phase. X-ray diffraction analysis of the samples was carried out for the confirmation and determination of crystal structure of the material. Data obtained from X-ray diffraction analysis helped in determining various parameters of the samples like lattice parameters, volume of the unit cell, crystallite size, bulk density of the samples, X-ray density and porosity of the samples.Keywords:Ferrites; Sol-gel method; X-Ray diffraction; Crystal structure.© 2013 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved.doi: http://dx.doi.org/10.3329/jsr.v5i2.11578           J. Sci. Res. 5 (2), 235-244 (2013)

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

scholarly journals Deep learning for visualization and novelty detection in large X-ray diffraction datasets

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Lars Banko ◽  
Phillip M. Maffettone ◽  
Dennis Naujoks ◽  
Daniel Olds ◽  
Alfred Ludwig
Keyword(s):  
Thin Film ◽  
Crystal Structure ◽  
Artificial Intelligence ◽  
Deep Learning ◽  
Novelty Detection ◽  
Structural Similarity ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Patterns ◽  
Post Hoc

AbstractWe apply variational autoencoders (VAE) to X-ray diffraction (XRD) data analysis on both simulated and experimental thin-film data. We show that crystal structure representations learned by a VAE reveal latent information, such as the structural similarity of textured diffraction patterns. While other artificial intelligence (AI) agents are effective at classifying XRD data into known phases, a similarly conditioned VAE is uniquely effective at knowing what it doesn’t know: it can rapidly identify data outside the distribution it was trained on, such as novel phases and mixtures. These capabilities demonstrate that a VAE is a valuable AI agent for aiding materials discovery and understanding XRD measurements both ‘on-the-fly’ and during post hoc analysis.

scholarly journals Born out of Fire and Ice: Polymorph Studies of the Antiviral Famciclovir

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Variable Temperature ◽  
Chemical Properties ◽  
Crystal Form ◽  
X Ray Diffraction ◽  
Crystal Forms ◽  
X Ray ◽  
Physical Chemical ◽  
Diffraction Patterns ◽  
Crystalline Forms

There is much interest and focus on solid forms of famciclovir. However, in spite of the abundance of reported differences in oral bioavailability, compressibility, and other physical–chemical properties of the various crystal forms of this drug, very little precise structural analysis is available in the literature to date. The form used in the commercial formulation is the anhydrous form I. Patents and patent applications report three different anhydrous crystalline forms on the basis of unindexed powder diffraction patterns. Single-crystal and variable-temperature X-ray diffraction experiments using the commercially available anhydrous form of famciclovir were carried out and led not only to the crystal structure determination of the anhydrous form I, but also to discovery of a new crystal form of anhydrous famciclovir from powder data.

CRYSTAL STRUCTURE OF ZIRCONIUM TRICHLORIDE

1964 ◽  
Vol 42 (10) ◽  
pp. 1886-1889 ◽  
Author(s):  
B. Swaroop ◽  
S. N. Flengas
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Main Cell ◽  
Diffraction Patterns

The crystal structure of zirconium trichloride was determined from X-ray diffraction patterns. Zirconium trichloride belongs to the [Formula: see text]space group. The dimensions of the main cell at room temperature are: a = 5.961 ± 0.005 Å and c = 9.669 ± 0.005 Å.The density of zirconium trichloride was measured and gave the value of 2.281 ± 0.075 g/cm3 while, from the X-ray calculations, the value was found to be 2.205 g/cm3.

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