The structure of poly(ethylene oxide)8 : NaBPh4 from a single crystal oligomer and polycrystalline polymerElectronic supplementary information (ESI) available: powder diffraction data for PEO8 : NaBPh4. See http://www.rsc.org/suppdata/cc/b3/b311800b/

2004 ◽  
pp. 148 ◽  
Author(s):  
Edward Staunton ◽  
Alasdair M. Christie ◽  
Yuri G. Andreev ◽  
Alexandra M. Z. Slawin ◽  
Peter G. Bruce
Keyword(s):  
Ethylene Oxide ◽  
Single Crystal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Supplementary Information ◽  
Powder Diffraction Data ◽  
Poly Ethylene Oxide ◽  
Poly Ethylene

Challenging structure determination from powder diffraction data: two pharmaceutical salts and one cocrystal with Z′ = 2

2019 ◽  
Vol 234 (4) ◽  
pp. 257-268 ◽  
Author(s):  
Carina Schlesinger ◽  
Michael Bolte ◽  
Martin U. Schmidt
Keyword(s):  
Single Crystal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Structure Determination ◽  
Real Space ◽  
Powder Diffraction Data ◽  
The Real ◽  
Pharmaceutical Salts ◽  
Structure Solution ◽  
Space Method

Abstract Structure solution of molecular crystals from powder diffraction data by real-space methods becomes challenging when the total number of degrees of freedom (DoF) for molecular position, orientation and intramolecular torsions exceeds a value of 20. Here we describe the structure determination from powder diffraction data of three pharmaceutical salts or cocrystals, each with four molecules per asymmetric unit on general position: Lamivudine camphorsulfonate (1, P 21, Z=4, Z′=2; 31 DoF), Theophylline benzamide (2, P 41, Z=8, Z′=2; 23 DoF) and Aminoglutethimide camphorsulfonate hemihydrate [3, P 21, Z=4, Z′=2; 31 DoF (if the H2O molecule is ignored)]. In the salts 1 and 3 the cations and anions have two intramolecular DoF each. The molecules in the cocrystal 2 are rigid. The structures of 1 and 2 could be solved without major problems by DASH using simulated annealing. For compound 3, indexing, space group determination and Pawley fit proceeded without problems, but the structure could not be solved by the real-space method, despite extensive trials. By chance, a single crystal of 3 was obtained and the structure was determined by single-crystal X-ray diffraction. A post-analysis revealed that the failure of the real-space method could neither be explained by common sources of error such as incorrect indexing, wrong space group, phase impurities, preferred orientation, spottiness or wrong assumptions on the molecular geometry or other user errors, nor by the real-space method itself. Finally, is turned out that the structure solution failed because of problems in the extraction of the integrated reflection intensities in the Pawley fit. With suitable extracted reflection intensities the structure of 3 could be determined in a routine way.

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.

Phase transformations in a double complex salt of the ruthenium nitrosyl anion and tetraamine-palladium cation

CrystEngComm ◽  
2020 ◽  
Vol 22 (21) ◽  
pp. 3692-3700
Author(s):  
G. A. Kostin ◽  
E. Yu. Filatov ◽  
D. P. Pischur ◽  
N. V. Kuratieva ◽  
S. V. Korenev
Keyword(s):  
Phase Transition ◽  
Single Crystal ◽  
Phase Transformations ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Complex Salt ◽  
Powder Diffraction Data ◽  
Double Complex ◽  
Disorder Phase Transition ◽  
Ruthenium Nitrosyl

A reversible order–disorder phase transition in [Pd(NH3)4][RuNO(NO2)4OH] in the temperature range of 370–390 K was confirmed by DSC, single crystal and powder diffraction data.

X-ray powder diffraction data for estra-4,9-diene-3,17-dione, C18H22O2

2020 ◽  
Vol 35 (4) ◽  
pp. 282-285
Author(s):  
Zhicheng Zha ◽  
Ting Tang ◽  
Xiaoyan Bian ◽  
Qing Wang
Keyword(s):  
Single Crystal ◽  
Cell Volume ◽  
Powder Diffraction ◽  
Structure Data ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Space Group ◽  
X Ray

X-ray powder diffraction data for estra-4,9-diene-3,17-dione, C18H22O2, are reported [a = 9.236(7) Å, b = 10.294(4) Å, c = 15.471(1) Å, unit cell volume V = 1471.11 Å3, Z = 4, and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurities were observed. The single-crystallographic data of the compound are also reported [a = 9.2392(7) Å, b = 10.2793(5) Å, c = 15.4822(7) Å, unit cell volume V = 1470.37(15) Å3, Z = 4, and space group P212121]. Both single-crystal and powder diffraction methods can get the similar structure data.

scholarly journals Reinvestigation of trilithium divanadium(III) tris(orthophosphate), Li3V2(PO4)3, based on single-crystal X-ray data

2013 ◽  
Vol 69 (2) ◽  
pp. i11-i12 ◽  
Author(s):  
Yongho Kee ◽  
Hoseop Yun
Keyword(s):  
Single Crystal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Title Compound ◽  
Three Dimensional ◽  
Structure Type ◽  
Powder Diffraction Data ◽  
Charge Balance ◽  
X Ray ◽  
Anisotropic Displacement Parameters

The structure of Li3V2(PO4)3has been reinvestigated from single-crystal X-ray data. Although the results of the previous studies (all based on powder diffraction data) are comparable with our redetermination, all atoms were refined with anisotropic displacement parameters in the current study, and the resulting bond lengths are more accurate than those determined from powder diffraction data. The title compound adopts the Li3Fe2(PO4)3structure type. The structure is composed of VO6octahedra and PO4tetrahedra by sharing O atoms to form the three-dimensional anionic framework∞3[V2(PO4)3]3−. The positions of the Li+ions in the empty channels can vary depending on the synthetic conditions. Bond-valence-sum calculations showed structures that are similar to the results of the present study seem to be more stable compared with others. The classical charge balance of the title compound can be represented as [Li+]3[V3+]2[P5+]3[O2−]12.

Arrangement of Rh3+ions infac-triamminetrichloridorhodium from powder data and infac-triamminetrinitratorhodium crystals twinned by merohedry

2013 ◽  
Vol 69 (12) ◽  
pp. 1462-1466 ◽  
Author(s):  
Alexander D. Vasiliev ◽  
Maxim S. Molokeev ◽  
Iraida A. Baidina ◽  
Anatoly V. Belyaev ◽  
Sofiya N. Vorob'eva
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rhodium Complexes ◽  
Powder Diffraction Data ◽  
Threefold Axis ◽  
Solubility In Water ◽  
Using Data ◽  
Low Solubility

The rhodium complexes [RhCl3(NH3)3], (I), and [Rh(NO3)3(NH3)3], (II), are built from octahedral RhX3(NH3)3units; in (I) they are isolated units, while in (II) the units are stacked in columns with partially filled sites for the Rh atoms. The octahedra of monoclinic crystals of (I) are linked by N—H...Cl hydrogen bonds and the Rh3+ions are located on the mirror planes. In the trigonal crystals of (II), the discontinuous `columns' along the threefold axis are linked by N—H...O hydrogen bonds. The structure of (I) has been solved using laboratory powder diffraction data, the structure of (II) has been solved by single-crystal methods using data from a merohedrally twinned sample. Both compounds possess low solubility in water.

On racemic and L-malates: a comparison of their crystal structures

2004 ◽  
Vol 219 (2) ◽  
Author(s):  
Michel Fleck ◽  
Ekkehart Tillmanns ◽  
Ladislav Bohatý ◽  
Peter Held
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Powder Diffraction File ◽  
Space Group ◽  
X Ray

AbstractThe crystal structures of eight different L-malates have been determined and refined from single-crystal X-ray diffraction data. The compounds are the monoclinic (space groupIn addition, for all the compounds, powder diffraction data were collected, analysed and submitted to the powder diffraction file (PDF).

Calculation of Single-Crystal Elastic Constants for Cubic Crystal Symmetry from Powder Diffraction Data

1998 ◽  
Vol 31 (6) ◽  
pp. 929-935 ◽  
Author(s):  
Thomas Gnäupel-Herold ◽  
Paul C. Brand ◽  
Henry J. Prask
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Powder Diffraction ◽  
Elastic Constants ◽  
Diffraction Data ◽  
Lattice Strain ◽  
Strain Response ◽  
Powder Diffraction Data ◽  
Cubic Crystal ◽  
Cubic Symmetry

In this work a method is developed that allows the computation of the single-crystal elastic constants for crystals of cubic symmetry from the diffraction elastic constants. The diffraction elastic constants can be obtained by measuring thehkl-dependent lattice strain response to an applied stress. Because of theirhkldependence they represent, partially, the anisotropic nature of the single-crystal elastic constants. The computation of the single-crystal elastic constants is carried out by a least-squares refinement which fits the calculated diffraction elastic constants to the measured ones.

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