Structures of three substituted arenesulfonamides from X-ray powder diffraction data using the differential evolution technique

2002 ◽  
Vol 58 (5) ◽  
pp. 823-834 ◽  
Author(s):  
Maryjane Tremayne ◽  
Colin C. Seaton ◽  
Christopher Glidewell
Keyword(s):  
Hydrogen Bonds ◽  
Differential Evolution ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Three Dimensional ◽  
Differential Evolution Algorithm ◽  
Space Structure ◽  
Powder Diffraction Data ◽  
X Ray

The structures of three substituted arenesulfonamides have been solved from laboratory X-ray powder diffraction data, using a new direct-space structure solution method based on a differential evolution algorithm, and refined by the Rietveld method. In 2-toluenesulfonamide, C7H9NO2S (I) (tetragonal I41/a, Z = 16), the molecules are linked by N—H...O=S hydrogen bonds into a three-dimensional framework. In 3-nitrobenzenesulfonamide, C6H6N2O4S (II) (monoclinic P21, Z = 2), N—H...O=S hydrogen bonds produce molecular ladders, which are linked into sheets by C—H...O=S hydrogen bonds: the nitro group does not participate in the hydrogen bonding. Molecules of 4-nitrobenzenesulfonamide, C6H6N2O4S (III) (monoclinic P21/n, Z = 4), are linked into sheets by four types of hydrogen bond, N—H...O=S, N—H...O(nitro), C—H...O=S and C—H...O(nitro), and the sheets are weakly linked by aromatic π...π stacking interactions.

X-ray powder diffraction data and Rietveld refinement for Ln6WO12 (Ln=Y, Ho)

2000 ◽  
Vol 15 (4) ◽  
pp. 220-226 ◽  
Author(s):  
N. Diot ◽  
P. Bénard-Rocherullé ◽  
R. Marchand
Keyword(s):  
Rare Earth ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Three Dimensional ◽  
Fluorite Structure ◽  
Rhombohedral Structure ◽  
Powder Diffraction Data ◽  
Tungsten Atom ◽  
X Ray

The crystal structure of the two isostructural rare earth tungstates Ln6WO12 (Ln=Y, Ho) has been refined by the Rietveld method from X-ray powder diffraction data. They crystallize with a three-dimensional rhombohedral structure (S.G. R3¯ and Z=3 for the R-centered setting) closely related to that of the binary oxides Ln7O12 and deriving from the ideal fluorite structure. Final refinements, with isotropic thermal motion for each atom, resulted in profile and structure factors Rwp=0.166, RF=0.037 with Ln=Y and Rwp=0.121, RF=0.040 with Ln=Ho. The rare earth element is sevenfold coordinated with Ln–O bond lengths ranging from 2.19 to 2.70 Å for Y6WO12 and from 2.18 to 2.68 Å for Ho6WO12; the coordination polyhedron may be described as a monocapped trigonal prism. The tungsten atom is located at the center of a WO6 octahedron with a unique W–O distance of 1.98 and 1.92 Å for Y6WO12 and Ho6WO12, respectively.

Structure of [Pd(NH3)4]Cr2O7

1995 ◽  
Vol 10 (3) ◽  
pp. 159-164 ◽  
Author(s):  
Y. Laligant ◽  
A. Le Bail
Keyword(s):  
Hydrogen Bonds ◽  
Ab Initio ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray

The structure of [Pd(NH3)4]Cr2O7 has been determined ab initio from conventional X-Ray powder diffraction data by the Patterson method. The cell is monoclinic (space group P21/c, Z = 4), with a = 7.771(3) Å, b=11.578(1) Å, c=11.852(4) Å, and β= 105.50(4)°. Refinements of 57 parameters by the Rietveld method, using 852 reflections lead to RB = 0.032, RP = 0.075, and Rwp = 0.092. The structure is built up from PdN4 square planes linked to Cr2O7 groups by hydrogen bonds. Hydrogen atoms could not be located.

Crystallographic study of ternary ordered skutterudite IrGe1.5Se1.5

2010 ◽  
Vol 25 (3) ◽  
pp. 247-252 ◽  
Author(s):  
F. Laufek ◽  
J. Návrátil
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Crystallographic Data ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Crystallographic Study ◽  
Related Phase ◽  
The Ideal

The crystal structure of skutterudite-related phase IrGe1.5Se1.5 has been refined by the Rietveld method from laboratory X-ray powder diffraction data. Refined crystallographic data for IrGe1.5Se1.5 are a=12.0890(2) Å, c=14.8796(3) Å, V=1883.23(6) Å3, space group R3 (No. 148), Z=24, and Dc=8.87 g/cm3. Its crystal structure can be derived from the ideal skutterudite structure (CoAs3), where Se and Ge atoms are ordered in layers perpendicular to the [111] direction of the original skutterudite cell. Weak distortions of the anion and cation sublattices were also observed.

Rietveld Refinement of the BaTiO3 from X-Ray Powder Diffraction

2009 ◽  
Vol 79-82 ◽  
pp. 593-596
Author(s):  
Feng Sun ◽  
Yan Sheng Yin
Keyword(s):  
Rietveld Refinement ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Structural Parameters ◽  
Ferroelectric Ceramic ◽  
Powder Diffraction Data ◽  
Ceramic Powders ◽  
Space Group ◽  
X Ray

The ferroelectric ceramic BaTiO3 was synthesized at 1000 °C for 5 h. The structure of the system under study was refined on the basis of X-ray powder diffraction data using the Rietveld method. The system crystallizes in the space group P4mm（99）. The refinement of instrumental and structural parameters led to reliable values for the Rp, Rwp and Rexp.We use the TOPAS software of Bruker AXS to refine this ceramic powders and show its conformation

scholarly journals Crystal structure from X-ray powder diffraction data, DFT-D calculation, Hirshfeld surface analysis, and energy frameworks of (RS)-trichlormethiazide

2022 ◽  
Vol 78 (2) ◽  
Author(s):  
Robert A. Toro ◽  
Analio Dugarte-Dugarte ◽  
Jacco van de Streek ◽  
José Antonio Henao ◽  
José Miguel Delgado ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Surface Analysis ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Electrostatic Interactions ◽  
Hirshfeld Surface ◽  
Hirshfeld Surface Analysis ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Π Interactions

The structure of racemic (RS)-trichlormethiazide [systematic name: (RS)-6-chloro-3-(dichloromethyl)-1,1-dioxo-3,4-dihydro-2H-1λ6,2,4-benzothiadiazine-7-sulfonamide], C8H8Cl3N3O4S2 (RS-TCMZ), a diuretic drug used in the treatment of oedema and hypertension, was determined from laboratory X-ray powder diffraction data using DASH [David et al. (2006). J. Appl. Cryst. 39, 910–915.], refined by the Rietveld method with TOPAS-Academic [Coelho (2018). J. Appl. Cryst. 51, 210–218], and optimized using DFT-D calculations. The extended structure consists of head-to-tail dimers connected by π–π interactions which, in turn, are connected by C—Cl...π interactions. They form chains propagating along [101], further connected by N—H...O hydrogen bonds to produce layers parallel to the ac plane that stack along the b-axis direction, connected by additional N—H...O hydrogen bonds. The Hirshfeld surface analysis indicates a major contribution of H...O and H...Cl interactions (32.2 and 21.7%, respectively). Energy framework calculations confirm the major contribution of electrostatic interactions (E elec) to the total energy (E tot). A comparison with the structure of S-TCMZ is also presented.

Structure Refinements of the Layered Intergrowth Phases SbIIISbV x A 1−x TiO6 (x≃0, A = Ta, Nb) Using Synchrotron X-ray Powder Diffraction Data

1997 ◽  
Vol 53 (6) ◽  
pp. 861-869 ◽  
Author(s):  
C. D. Ling ◽  
J. G. Thompson ◽  
S. Schmid ◽  
D. J. Cookson ◽  
R. L. Withers
Keyword(s):  
Single Crystal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Homologous Series ◽  
Rietveld Method ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Synchrotron Source ◽  
X Ray ◽  
The Family

The structures of the layered intergrowth phases SbIIISb^{\rm V}_xAl-xTiO6 (x \simeq 0, A = Ta, Nb) have been refined by the Rietveld method, using X-ray diffraction data obtained using a synchrotron source. The starting models for these structures were derived from those of Sb^{\rm III}_3Sb^{\rm V}_xA 3−xTiO14 (x = 1.26, A = Ta and x = 0.89, A = Nb), previously solved by single-crystal X-ray diffraction. There were no significant differences between the derived models and the final structures, validating the approach used to obtain the models and confirming that the n = 1 and n = 3 members of the family, Sb^{\rm III}_nSb^{\rm V}_xA n−xTiO4n+2 are part of a structurally homologous series.

Two polymorphs of 2-ethyl-3-hydroxy-6-methylpyridinium hydrogenN-acetyl-L-glutamate from powder diffraction data

2013 ◽  
Vol 69 (12) ◽  
pp. 1549-1552 ◽  
Author(s):  
Vladimir V. Chernyshev ◽  
Sergey Y. Efimov ◽  
Ksenia A. Paseshnichenko ◽  
Andrey A. Shiryaev
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Crystal Packing ◽  
Three Dimensional ◽  
Powder Diffraction Data ◽  
Screw Axis ◽  
Dimensional Network ◽  
Polymorphic Modifications

The title salt, C8H12NO+·C7H10NO5−, crystallizes in two polymorphic modifications,viz.monoclinic (M) and orthorhombic (O). The crystal structures of both polymorphic modifications have been established from laboratory powder diffraction data. The crystal packing motifs in the two polymorphs are different, but the conformations of the anions are generally similar. InM, the anions are linked by pairs of hydrogen bonds of the N—H...O and O—H...O types into chains along theb-axis direction, and neighbouring molecules within the chain are related by the 21screw axis. The cations link these chainsviaO—H...O and N—H...O hydrogen bonds into layers parallel to (001). InO, the anions are linked by O—H...O hydrogen bonds into helices along [001], and neighbouring molecules within the helix are related by the 21screw axis. The neighbouring helical turns are linked by N—H...O hydrogen bonds. The cations link the helicesviaO—H...O and N—H...O hydrogen bonds, thus forming a three-dimensional network.

scholarly journals Quantitative Phase Analysis of Skarn Rocks by the Rietveld Method Using X-ray Powder Diffraction Data

Minerals ◽  
2020 ◽  
Vol 10 (10) ◽  
pp. 894
Author(s):  
Yana Tzvetanova ◽  
Ognyan Petrov ◽  
Thomas Kerestedjian ◽  
Mihail Tarassov
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Rietveld Analysis ◽  
Quantitative Phase Analysis ◽  
Chemical Compositions ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Fine Grained ◽  
Variable Chemical

The Rietveld method using X-ray powder diffraction data was applied to selected skarn samples for quantitative determination of the present minerals. The specimens include garnet, clinopyroxene–garnet, plagioclase–clinopyroxene–wollastonite–garnet, plagioclase–clinopyroxene–wollastonite, plagioclase–clinopyroxene–wollastonite–epidote, and plagioclase–clinopyroxene skarns. The rocks are coarse- to fine-grained and characterized by an uneven distribution of the constituent minerals. The traditional methods for quantitative analysis (point-counting and norm calculations) are not applicable for such inhomogeneous samples containing minerals with highly variable chemical compositions. Up to eight individual mineral phases have been measured in each sample. To obtain the mineral quantities in the skarn rocks preliminary optical microscopy and chemical investigation by electron probe microanalysis (EPMA) were performed for the identification of some starting components for the Rietveld analysis and to make comparison with the Rietveld X-ray powder diffraction results. All of the refinements are acceptable, as can be judged by the standard indices of agreement and by the visual fits of the observed and calculated diffraction profiles. A good correlation between the refined mineral compositions and the data of the EPMA measurements was achieved.

Structure Refinement of High-Density Polyethylene Using X-Ray Powder Diffraction Data and the Rietveld Method

1995 ◽  
Vol 39 ◽  
pp. 515-521
Author(s):  
Kenneth B. Schwartz ◽  
Robert B. Von Dreele
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
High Density Polyethylene ◽  
Rietveld Method ◽  
Structure Refinement ◽  
High Density ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Voigt Profile ◽  
Full Structure

A full structure analysis of a completely crystallized sample of high-density polyethylene (HDPE) has been achieved using x-ray powder diffraction data collected on a laboratory-based powder diffractometer. The structure refinement is performed using the Rietveld method and includes refinement of the carbon and hydrogen atomic positions and temperature factors. The C-C and C-H bond distances and the C-C-C bond angle along the polyethylene chain have been calculated from the refined atomic positions and are in very good agreement with previous experimental and modelling determinations. Evaluations of the pseudo-Voigt profile parameters for Lorentzian strain broadening and me Scherrer coefficient for Gaussian broadening yield reasonable values for microstrain and particle size for this sample. Refinement of the preferred orientation parameter indicates that the HDPE flakes consist of platy crystals or lamellae that are packed normal to the diffraction vector.

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