Parametric Rietveld refinement.
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ABSTRACT:
SUBMITTER: Stinton GW
PROVIDER: S-EPMC2483475 | biostudies-literature |
REPOSITORIES: biostudies-literature
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Project description:Y(2)GeO(5) (yttrium germanium penta-oxide) was synthesized by solid-state reaction at 1443?K. The arrangement, which has monoclinic symmetry, is isostructural with Dy(2)GeO(5) and presents two independent sites for the Y atoms. Around these atoms there are distorted six-coordinated YO(6) octa-hedra and seven-coordinated YO(7) penta-gonal bipyramids. The YO(7) polyhedra are linked together, sharing their edges along a surface parallel to ab, forming a sheet. Each of these parallel sheets is inter-connected by means of GeO(4) tetra-hedra, sharing an edge (or vertex) on one side and a vertex (or edge) on the other adjacent side. Parallel sheets of YO(7) polyhedra are also inter-connected by undulating chains of YO(6) octa-hedra along the c axis. These octa-hedra are joined together, sharing a common edge, to form the chain and share edges with the YO(7) polyhedra of the sheets.
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Project description:This study aims to solve the site-occupancy issues of any crystalline substance, showing that the structure refinement results should not be limited to a simple description of the crystal geometry but should go beyond that, providing refined site-scattering values consistent with the chemical data. A detailed description of the structure of the amphibole-supergroup minerals is very challenging owing to their complex chemical composition that renders the process of cation partition extremely difficult, particularly because of the occurrence of multivalent elements. Since amphiboles naturally occur under a fibrous morphology and have largely been used to produce asbestos, there is a growing demand for detailed and accurate structural data in order to study the relationships between structure, composition and toxicity. The present study proposes a recommended refinement procedure for both X-ray single-crystal structure refinement (SREF) and Rietveld analysis for tremolite, selected as a test case. The corresponding structural results are compared to estimate the ‘degree of confidence’ of the Rietveld refinement with regard to SREF. In particular, it is shown that the interpretation of the electron density of the tremolite structure by SREF is model dependent. By assuming that the site-scattering values from SREF should be as close as possible to those from electron microprobe analysis, as a crucial constraint for the correct description of the final crystal-chemical model, it is found that it is best satisfied by using partially ionized scattering curves (SCs) for O and Si, and neutral SCs (neutral oxygen curves or NOCs) for other atoms. This combination leads to the best fit to the diffraction data. Moreover, it is found that Rietveld refinement using NOCs produces the best structural results, in excellent agreement with SREF. It is worth noting that, due to the complexity of the diffraction pattern and the fairly large number of freely refinable parameters, refinements with different combinations of SCs produce results almost indistinguishable from a statistical point of view, albeit showing significant differences from a structural point of view.
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Project description:A structural refinement of a natural sample of a Co-bearing mansfieldite, AlAsO(4)·2H(2)O [aluminium orthoarsenate(V) dihydrate], has been performed based on synchrotron powder diffraction data, with 5% of the octa-hedral Al sites replaced by Co. Mansfieldite is the aluminium analogue and an isotype of the mineral scorodite (FeAsO(4)·2H(2)O), with which it forms a solid solution. The framework structure is based on AsO(4) tetra-hedra sharing their vertices with AlO(4)(H(2)O)(2) octa-hedra. Three of the four H atoms belonging to the two water mol-ecules in cis positions take part in O-H?O hydrogen bonding.
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Project description:Potassium lanthanum titanate(IV), KLaTiO(4), has been synthesized by conventional solid-state reaction. It crystallizes isotypically with the NaLnTiO(4) (Ln = La, Pr, Nd, Sm, Eu, Gd, Y and Lu) family. Five of the six atoms in the asymmetric unit (one K, one La, one Ti and two O atoms) are situated on sites with 4mm symmetry, whereas one O atom has 2mm. site symmetry. The crystal structure can be described as being composed of single layers of distorted corner-sharing TiO(6) octa-hedra extending parallel to (001). The layers are alternately separated by K(+) and La(3+) cations along [001]. The coordination number of both K(+) and La(3+) cations is nine, resulting in distorted KO(9) and LaO(9) polyhedra.
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Project description:Polycrystalline silver(I) deca-calcium heptakis(orthophos-phate), AgCa10(PO4)7, was obtained by solid-state reaction. It is isotopic with members of the series MCa10(PO4)7 (M = Li, Na, K and Cs), and is closely related to the structure of ?-Ca3(PO4)2. The crystal structure of the title compound is built up from a framework of [CaO9] and two [CaO8] polyhedra, one [CaO6] octa-hedron (site symmetry 3.) and three PO4 tetra-hedra (one with site symmetry 3.). The Ag(+) cation is likewise located on a threefold rotation axis and resides in the cavities of the rigid [Ca10(PO4)7](-) framework. It is surrounded by three O atoms in an almost regular triangular environment.
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Project description:Dipotassium [nickel(II) zirconium(IV)] tris-(orthophosphate) was prepared from a self-flux in the system K2O-P2O5-NiO-K2ZrF6. The title compound belongs to the langbeinite family and is built up from two [MO6] octa-hedra [M = Ni:Zr with mixed occupancy in ratios of 0.21?(4):0.79?(4) and 0.29?(4):0.71?(4), respectively] and [PO4] tetra-hedra inter-linked via vertices into a (3) ?[M 2(PO4)3] framework. Two independent K(+) cations are located in large cavities of the framework, with coordination numbers to O(2-) anions of nine and twelve. The K, Ni, and Zr sites are located on threefold rotation axes.
| S-EPMC4120588 | biostudies-literature
Project description:The synthetic leucite silicate framework mineral analogues Rb2 XSi5O12 {X = Ni [dirubidium nickel(II) penta-silicate] and Mn [dirubidium manganese(II) penta-silicate]} have been prepared by high-temperature solid-state synthesis. The results of Rietveld refinements, using X-ray powder diffraction data collected using Cu Kα X-rays, show that the title compounds crystallize in the space group Pbca and adopt the cation-ordered structure of Cs2CdSi5O12 and other leucites. The structures consist of tetra-hedral SiO4 and XO4 units sharing corners to form a partially substituted silicate framework. Extraframework Rb(+) cations sit in channels in the framework. All atoms occupy the 8c general position for this space group. In these refined structures, silicon and X atoms are ordered onto separate tetra-hedrally coordinated sites (T-sites). However, the Ni displacement parameter and the Ni-O bond lengths suggest that for the X = Ni sample, there may actually be some T-site cation disorder.
| S-EPMC4770953 | biostudies-literature
Project description:Potassium yttrium hafnium tris-(orthophosphate) belongs to the langbeinite-family and is built up from [MO(6)] octa-hedra [in which the positions of the two independent M sites are mutually occupied by Y and Hf in a 0.605?(10):0.395?(10) ratio] and [PO(4)] tetra-hedra connected via vertices into a three-dimensional framework. This framework is penetrated by large closed cavities in which the two independent K atoms are located; one of the K atoms is nine-coordinated and the other is 12-coordinated by surrounding O atoms. The K, Y and Hf atoms lie on threefold rotation axes, whereas the P and O atoms are located in general positions.
| S-EPMC2977454 | biostudies-other
Project description:The title compound, K(0.8)Ca(9.8)Fe(0.2)(PO(4))(7) (potassium deca-calcium iron hepta-phosphate), belongs to the whitlockite family. The structure is built up from several types of metal-oxygen polyhedra: two [CaO(8)], one [CaO(7)] and one [(Ca/Fe)O(6)] polyhedron with a mixed Ca/Fe occupancy in a 0.8:0.2 ratio, as well as three tetra-hedral [PO(4)] units. Of the 18 sites in the asymmetric unit, the site with the mixed Ca/Fe occupation, the K site, one P and one O site are on special positions 6a with 3 symmetry, whereas all other sites are on general positions 18b. The linkage of metal-oxygen polyhedra and [PO(4)] tetra-hedra via edges and corners results in formation of a three-dimensional framework with composition [Ca(9.8)Fe(0.2)(PO(4))(7)](0.8-). The remaining K atoms (site-occupation factor = 0.8) are located in large closed cavities and are nine-coordinated by oxygen.
| S-EPMC2979107 | biostudies-literature
Project description:The apatite-type compound Ba(5)(AsO(4))(3)Cl, penta-barium tris-[arsenate(V)] chloride, has been synthesized by ion exchange at high temperature from a synthetic sample of mimetite (Pb(5)(AsO(4))(3)Cl) with BaCO(3) as a by-product. The results of the Rietveld refinement, based on high resolution synchrotron X-ray powder diffraction data, show that the title compound crystallizes in the same structure as other halogenoapatites with general formula A(5)(YO(4))(3)X (A = divalent cation, Y = penta-valent cation, X = Cl, Br) in space group P6(3)/m. The structure consists of isolated tetra-hedral AsO(4) (3-) anions (m symmetry), separated by two crystallographically independent Ba(2+) cations that are located on mirror planes and threefold rotation axes, respectively. The Cl(-) anions are at the 2b sites ( symmetry) and are located in the channels of the structure.
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