A new structure type in the hexagonal perovskite family; structure determination of the modulated misfit compound Sr9/8TiS3

2000 ◽  
Vol 56 (3) ◽  
pp. 409-418 ◽  
Author(s):  
O. Gourdon ◽  
V. Petricek ◽  
M. Evain
Keyword(s):  
Family Structure ◽  
Three Dimensional ◽  
Structure Type ◽  
X Ray ◽  
3D Space ◽  
Titanium Sulfide ◽  
New Type ◽  
New Phase ◽  
Trigonal Prismatic

Sr9/8TiS3, strontium titanium sulfide, a new phase in the hexagonal perovskite-like Sr x TiS3 system, has been prepared and its structure solved from single-crystal X-ray data within the (3 + 1)-dimensional [(3 + 1)D] formalism. Sr9/8TiS3 crystallizes with trigonal symmetry [R3¯m(00γ)0s superspace group], with the following lattice parameters: a s = 11.482 (3), c s = 2.9843 (8) Å, q = 0.56247 (7)c* and V s = 340.7 (3) Å3. The structure was considered as commensurate [R3¯c three-dimensional (3D) space group], but refined within the (3 + 1)D formalism to a residual factor R = 2.79% for 64 parameters and 1084 independent reflections. Original crenel functions were used for the sulfur and strontium description. The structure is different from that of the hexagonal perovskite-like oxide counterparts. The main difference is related to the presence of a new type of polyhedron in the [MS3] transition metal chains, intermediate between the octahedra classically found in such chains and the trigonal prismatic sites encountered in the oxides.

scholarly journals Determination of the Three-dimensional Structure of Dislocations by Synchrotron White X-ray Topography Combined with a Topo-tomographic Technique

Materia Japan ◽  
2007 ◽  
Vol 46 (12) ◽  
pp. 823-823
Author(s):  
Seiji Kawado ◽  
Toshinori Taishi ◽  
Satoshi Iida ◽  
Yoshifumi Suzuki ◽  
Yoshinori Chikaura ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Dimensional Structure ◽  
X Ray ◽  
Three Dimensional Structure ◽  
Tomographic Technique

scholarly journals Rubidium tetrafluoridobromate(III): redetermination of the crystal structure from single-crystal X-ray diffraction data

IUCrData ◽  
2019 ◽  
Vol 4 (11) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
Atomic Coordinates

Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].

X-ray topographic determination of the granular structure in a graphite mosaic crystal: a three-dimensional reconstruction

2000 ◽  
Vol 33 (4) ◽  
pp. 1023-1030 ◽  
Author(s):  
M. Ohler ◽  
M. Sanchez del Rio ◽  
A. Tuffanelli ◽  
M. Gambaccini ◽  
A. Taibi ◽  
...  
Keyword(s):  
Structural Parameters ◽  
Pyrolytic Graphite ◽  
Three Dimensional ◽  
X Ray ◽  
Dimensional Reconstruction ◽  
Mosaic Crystals ◽  
Spatial Locations ◽  
Crystalline Domains

Section topographs recorded at different spatial locations and at different rocking angles of a highly oriented pyrolytic graphite (HOPG) crystal allow three-dimensional maps of the local angular-dependent scattering power to be obtained. This is performed with a direct reconstruction from the intensity distribution on such topographs. The maps allow the extraction of information on local structural parameters such as size, form and internal mosaic spread of crystalline domains. This data analysis leads to a new method for the characterization of mosaic crystals. Perspectives and limits of applicability of this method are discussed.

Ternary Thallides REMgTl (Re = Y, La – Nd, Sm, Gd – Tm, Lu)

2005 ◽  
Vol 60 (3) ◽  
pp. 265-270 ◽  
Author(s):  
Rainer Kraft ◽  
Rainer Pöttgen
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Rare Earth Metal ◽  
High Frequency ◽  
Three Dimensional ◽  
Earth Metal ◽  
X Ray ◽  
Sample Chamber ◽  
Trigonal Prismatic Coordination ◽  
Trigonal Prismatic

The rare earth metal (RE)-magnesium-thallides REMgTl (RE = Y, La-Nd, Sm, Gd-Tm, Lu) were prepared from the elements in sealed tantalum tubes in a water-cooled sample chamber of a high-frequency furnace. The thallides were characterized through their X-ray powder patterns. They crystallize with the hexagonal ZrNiAl type structure, space group P62m, with three formula units per cell. Four structures were refined from X-ray single crystal diffractometer data: α = 750.5(1), c = 459.85(8) pm, wR2 = 0.0491, 364 F2 values, 14 variables for YMgTl; α = 781.3(1), c = 477.84(8) pm, wR2 = 0.0640, BASF = 0.09(2), 425 F2 values, 15 variables for LaMgTl; α = 774.1(1), c = 473.75(7) pm, wR2 = 0.0405, 295 F2 values, 14 variables for CeMgTl; a = 760.3(1), c = 465.93(8) pm, wR2 = 0.0262, 287 F2 values, 14 variables for SmMgTl. The PrMgTl, NdMgTl, GdMgTl, TbMgTl, and DyMgTl structures have been analyzed using the Rietveld technique. The REMgTl structures contain two cystallographically independent thallium sites, both with tri-capped trigonal prismatic coordination: Tl1Mg3RE6 and Tl2Mg6RE3. Together the magnesium and thallium atoms form three-dimensional [MgTl] networks with Mg-Mg distances of 327 and Mg-Tl distances in the range 299 - 303 pm (data for CeMgTl)

Sr4Pt10In21 – the first representative of the Ho4Ni10In21 type with a divalent cation

2019 ◽  
Vol 74 (5) ◽  
pp. 443-449 ◽  
Author(s):  
Birgit Heying ◽  
Jutta Kösters ◽  
Rainer Pöttgen
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Glassy Carbon ◽  
Divalent Cation ◽  
High Frequency ◽  
Three Dimensional ◽  
X Ray ◽  
Trigonal Prismatic Coordination ◽  
Trigonal Prismatic

AbstractRod-shaped single crystals of Sr4Pt10In21were prepared from the elements in glassy-carbon crucibles in a high-frequency furnace. The structure of Sr4Pt10In21was refined from single-crystal X-ray diffractometer data:C2/m, Ho4Ni10Ga21type,a = 2322.62(7),b = 450.27(2),c = 1958.09(7) pm,β = 133.191(3)°,wR = 0.0464, 3200F2values and 107 variables. The three-dimensional [Pt10In21]δ−polyanionic network is stabilized through substantial Pt–In (269–313 pm Pt–In) and In–In (294–362 pm In–In) bonding. All platinum atoms have slightly distorted tri-capped trigonal prismatic coordination and the two crystallographically independent strontium atoms are located in penta-capped pentagonal prisms.

scholarly journals Gold Exploration in Two and Three Dimensions: Improved and Correlative Insights from Microscopy and X-Ray Computed Tomography

Minerals ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 476
Author(s):  
Joshua Chisambi ◽  
Bjorn von der Heyden ◽  
Muofhe Tshibalanganda ◽  
Stephan Le Roux
Keyword(s):  
Computed Tomography ◽  
Spatial Distribution ◽  
Gold Mineralization ◽  
Three Dimensional ◽  
Three Dimensions ◽  
Low Grade ◽  
X Ray ◽  
3D Space ◽  
X Ray Computed ◽  
2D And 3D

In this contribution, we highlight a correlative approach in which three-dimensional structural/positional data are combined with two dimensional chemical and mineralogical data to understand a complex orogenic gold mineralization system; we use the Kirk Range (southern Malawi) as a case study. Three dimensional structures and semi-quantitative mineral distributions were evaluated using X-ray Computed Tomography (XCT) and this was augmented with textural, mineralogical and chemical imaging using Scanning Electron Microscopy (SEM) and optical microscopy as well as fire assay. Our results detail the utility of the correlative approach both for quantifying gold concentrations in core samples (which is often nuggety and may thus be misrepresented by quarter- or half-core assays), and for understanding the spatial distribution of gold and associated structures and microstructures in 3D space. This approach overlays complementary datasets from 2D and 3D analytical protocols, thereby allowing a better and more comprehensive understanding on the distribution and structures controlling gold mineralization. Combining 3D XCT analyses with conventional 2D microscopies derive the full value out of a given exploration drilling program and it provides an excellent tool for understanding gold mineralization. Understanding the spatial distribution of gold and associated structures and microstructures in 3D space holds vast potential for exploration practitioners, especially if the correlative approach can be automated and if the resultant spatially-constrained microstructural information can be fed directly into commercially available geological modelling software. The extra layers of information provided by using correlative 2D and 3D microscopies offer an exciting new tool to enhance and optimize mineral exploration workflows, given that modern exploration efforts are targeting increasingly complex and low-grade ore deposits.

Structure determination of a partially ordered layered silicate material with an NMR crystallography approach

2017 ◽  
Vol 73 (3) ◽  
pp. 184-190 ◽  
Author(s):  
Darren Henry Brouwer ◽  
Sylvian Cadars ◽  
Kathryn Hotke ◽  
Jared Van Huizen ◽  
Nicholas Van Huizen
Keyword(s):  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Three Dimensional ◽  
Layered Silicate ◽  
Silicate Layer ◽  
Silicate Material ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Crystallography

Structure determination of layered materials can present challenges for conventional diffraction methods due to the fact that such materials often lack full three-dimensional periodicity since adjacent layers may not stack in an orderly and regular fashion. In such cases, NMR crystallography strategies involving a combination of solid-state NMR spectroscopy, powder X-ray diffraction, and computational chemistry methods can often reveal structural details that cannot be acquired from diffraction alone. We present here the structure determination of a surfactant-templated layered silicate material that lacks full three-dimensional crystallinity using such an NMR crystallography approach. Through a combination of powder X-ray diffraction and advanced 29Si solid-state NMR spectroscopy, it is revealed that the structure of the silicate layer of this layered silicate material templated with cetyltrimethylammonium surfactant cations is isostructural with the silicate layer of a previously reported material referred to as ilerite, octosilicate, or RUB-18. High-field 1H NMR spectroscopy reveals differences between the materials in terms of the ordering of silanol groups on the surfaces of the layers, as well as the contents of the inter-layer space.

Ab initio structure determination of nanosized θ-KAlF4 with edge-sharing AlF6 octahedra

2009 ◽  
Vol 24 (3) ◽  
pp. 185-190 ◽  
Author(s):  
A. Le Bail
Keyword(s):  
Crystal Structure ◽  
Ab Initio ◽  
Fluorite Structure ◽  
Structure Type ◽  
Powder Diffraction Data ◽  
Orthorhombic Unit Cell ◽  
Common Edge ◽  
X Ray ◽  
Ab Initio Structure

θ-KAlF4 is a new nanosized potassium tetrafluoroaluminate metastable polymorph (13×18×55 nm3). The crystal structure is solved ab initio from X-ray powder diffraction data in direct space [orthorhombic unit cell with a=8.3242(3) Å, b=7.2502(3) Å, c=11.8875(4) Å, V=717.44(5) Å3, Z=8, and space group Pnma]. This new structure type, unique in the whole AIMIIIF4 family, is related to the fluorite structure and consists of AlF6 octahedra linked via a common edge forming a bioctahedral motif which is trans-connected through the corner-shared fluorine, resulting in the formation of infinite ladderlike double file of octahedra ([Al2F8]2−)n running along the b axis.

scholarly journals The preparation and characterization of SeCl3SbF6, improved syntheses of MCl3(As/Sb)F6 (M = S, Se), and the X-ray crystal structure determination of SeCl3AsF6 and a new phase of SBr3SbF6

1996 ◽  
Vol 74 (9) ◽  
pp. 1671-1681 ◽  
Author(s):  
Jack Passmore ◽  
Paul D. Boyle ◽  
Gabriele Schatte ◽  
Todd Way ◽  
T. Stanley Cameron
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Ft Raman Spectroscopy ◽  
New Phase ◽  
Ft Raman

Alternative and, in some cases, improved syntheses of the salts MX3(As/Sb)F6 (M = S, Se) and SCl3(SbCl6/AlCl4) are described. In addition, the synthesis of SeCl3SbF6 is reported. The compounds were characterized by FT–Raman spectroscopy and the X-ray crystal structures of SeCl3AsF6 (also 77Se NMR) and a new phase of SBr3SbF6 were determined. Crystals of SeCl3AsF6 and SBr3SbF6 are monoclinic, space group P21/c with [values for SBr3SbF6 in brackets] a = 7.678(1) [8.137(1)] Å, b = 9.380(3) [9.583(2)] Å, c = 11.920(3) [12.447(2)] Å, β = 98.19(2)° [97.36(1)]°, V = 849.72(3) [962.6(3)] Å3,z = 4, Dx = 2.925 [3.502] Mg m−3, R = 0.0525 [0.055], and Rw = 0.0554 [0.060] for 1151 [1472] observed reflections. Key words: MX3+ salts, FT–Raman spectroscopy, X-ray crystal structures of SeCl3AsF6, SBr3SbF6, and preparation of SeCl3SbF6.

Ternary Indides REMgIn (RE = Y, La–Nd, Sm, Gd–Tm, Lu). Synthesis, Structure and Magnetic Properties

2004 ◽  
Vol 59 (5) ◽  
pp. 513-518 ◽  
Author(s):  
Rainer Kraft ◽  
Martin Valldor ◽  
Daniel Kurowski ◽  
Rolf-Dieter Hoffmann ◽  
Rainer Pöttgen
Keyword(s):  
Magnetic Moments ◽  
Three Dimensional ◽  
Temperature Dependent ◽  
Variable Parameters ◽  
Magnetic Susceptibility Data ◽  
X Ray ◽  
Susceptibility Data ◽  
Sample Chamber ◽  
Trigonal Prismatic Coordination ◽  
Trigonal Prismatic

Abstract The equiatomic rare earth-magnesium-indium compounds REMgIn (RE = Y, La-Nd, Sm, Gd- Tm, Lu) were prepared from the elements in sealed tantalum tubes inside a water-cooled sample chamber of an induction furnace. All compounds were characterized through their X-ray powder patterns. They crystallize with the hexagonal ZrNiAl type structure, space group P6̄̄2m, with three formula units per cell. The structure of SmMgIn was refined from X-ray single crystal diffractometer data: a = 761.3(2), c = 470.3(1) pm, wR2 = 0.0429, 380 F2 values and 14 variable parameters. The DyMgIn, HoMgIn, and TmMgIn structures have been analyzed using the Rietveld technique. The REMgIn structures contain two cystallographically independent indium sites, both with tri-capped trigonal prismatic coordination: In1Sm6Mg3 and In2Mg6Sm3. Together the magnesium and indium atoms form a three-dimensional [MgIn] network with Mg-Mg distances of 320 and Mg-In distances in the range 294 - 299 pm. Temperature dependent magnetic susceptibility data show Curie-Weiss behavior for DyMgIn, HoMgIn, and TmMgIn with experimental magnetic moments of 11.0(1) μB/Dy atom, 10.9(1) μB/Ho atom, and 7.5(1) μB/Tm atom. The three compounds order antiferromagnetically at TN = 22(2) K (DyMgIn), 12(1) K (HoMgIn), and 3(1) K (TmMgIn).

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