A new interpretation and practical aspects of the direct-methods modulus sum function. VIII

2001

Since the first publication of the direct-methods modulus sum function [Rius (1993). Acta Cryst. A49, 406-409], the application of this function to a variety of situations has been shown in a series of seven subsequent papers. In this way, much experience about this function and its practical use has been gained. It is thought by the authors that it is now the right moment to publish a more complete study of this function which also considers most of this practical knowledge. The first part of the study relates, thanks to a new interpretation, this function to other existing phase-refinement functions, while the second shows, with the help of test calculations on a selection of crystal stru…

Synthesis and crystal structures of two novel triazolopyridine compounds solved by local L.S. minimizations from powder diffraction data

2014

The heteroaryl-substituted triazolopyridines 3-phenyl-7-(pyrazin-2-yl)-[1,2,3]triazolo[1,5-a]pyridine (2) and 3-[6-(pyridazin-3-yl)-pyridin-2-yl]-[1,2,3]triazolo[1,5-a]pyridine (4) have been synthesized and characterized (by HRMS, IR,1H and13C NMR, XRPD, melting point). The crystal structures have been solved from laboratory powder X-ray diffraction data with the direct-space strategy TALP for molecular compounds based on fast local least-squares minimizations. The crystal structure confirmed the formation of the tridentate compound4from a ring chain isomerization process. The almost planar arrangement of atoms in both the structures favors the presence of intermolecularπ–πinteractions, alt…

Quantitative X-Ray Powder Diffraction Analysis of Some Feldspars Used as Raw Material in Ceramics

2001

Crystal structure determination of 1-pentanol from low-temperature powder diffraction data by Patterson search methods

2005

5 pages.-- PACS: 61.66.Hq; 61.50.Lt

The crystal structure of 3,5-diisopropyl-4-nitropyrazole from X-ray powder diffraction data

2001

The crystal structure of 3,5-diisopropyl-4-nitropyrazole, 3c, has been determined by a Patterson Search method from laboratory X-ray powder diffraction data. The crystal data are: monoclinic symmetry with the unit-cell parameters aa 19:530O5U; ba 6:485O1U and ca 17:937O3U A; ba 100:32O1U8; space group I2/a ,C 9H15N3O2, Za 8, 293 K. After indexing the powder pattern by two methods, the unit-cell parameters found were refined by a least-squares technique. A whole pattern- fitting program was used to extract the integrated intensities. The structure was solved taking a related compound as a search model and the final Rietveld refinement converged to Rwpa 0.1971 and Rpa 0.1437. The structure pr…

The Bi sulfates from the Alfenza Mine, Crodo, Italy: An automatic electron diffraction tomography (ADT) study

2014

We report about three bismuth sulfates from mineralized quartz dikes from Alfenza (Crodo, Italy), two new phases and a rare mineral, cannonite, all growing on bismuthinite. The first new phase occurs as white, "hortensia-like" aggregates of pseudo-hexagonal platelets, with perfect basal cleavage, similar to 20 mu m wide and few micrometers thick. The approximate composition is Bi2O2(SO4), and cell parameters and symmetry, as determined by automatic diffraction tomography, are a = 22.0(4), b = 16.7(3), c = 15.9(3) angstrom, beta = 102.9(5)degrees, space group Pc or P2/c. A major stacking disorder is detected by HR-SEM images and electron diffraction data.The second new phase was detected onl…

Quantitative x-ray diffraction phase analysis of coarse airborne particulate collected by cascade impactor sampling

1997

Mineralogical composition of Castellon (Spanish Mediterranean coast) atmospheric aerosol was studied by X-ray diffraction by sampling with a cascade impactor without filters. Quantitative phase analysis of natural phases present in the atmospheric coarse aerosol was performed using a modified version of the computer program MENGE, that uses the standardless X-ray method developed by Rius for the quantitative analysis of multiphase mixtures, adapted for PC running. Presence of quartz, calcite and gypsum was identified in the atmospheric aerosol and we have quantified their amounts using the standardless method.

Structure Determination from Powder X-Ray Diffraction Data of a Hydrogen-Bonded Molecular Solid with Competing Ferromagnetic and Antiferromagnetic In…

1995

Von den Pulver-Röntgenbeugungsdaten zur Struktur eines Molekülkristalls mit Wasserstoffbrückenbindungen und konkurrierenden ferromagnetischen und ant…

1995

A tangent formula derived from Patterson-function arguments. VII. Solution of inorganic structures from powder data with accidental overlap

2000

Accidental overlap constitutes one of the principal limitations for the solution of crystal structures from powder diffraction data, since it reduces the number of available intensities for direct-methods application. In this work, the field of application of the direct-methods sum function is extended to cope with powder patterns with relatively large amounts of accidental overlap. This is achieved by refining not only the phases of the structure factors but also the estimated intensities of the severely overlapped peaks during the structure solution process. This procedure has been specifically devised for inorganic compounds with uncertain cell contents and with probable severe atomic di…

Application of delta recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes

2013

δ Recycling is a simple procedure for directly extracting phase information from Patterson-type functions [Rius (2012). Acta Cryst. A68, 399-400]. This new phasing method has a clear theoretical basis and was developed with ideal single-crystal X-ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507-513]. When combined with precession electron diffraction, it delivers quasi-kinematical intensity data even for complex inorganic compounds, so that single-crystal diffraction data of nanometric volumes are now availa…

Determination of Molecular Crystal Structures from X-Ray Powder Diffraction Data

1993

Synthesis and structural properties of hexaaza[5]helicene containing two [1,2,3]triazolo[1,5-a]pyridine moieties

2013

Abstract We have synthesized a novel hexaaza[5]helicene in a straightforward way from neocuproine. The crystal structure has been elucidated with direct-space strategy TALP which demonstrates the power of the powder X-ray diffraction technique. In this crystal structure it is possible to see an interplanar angle of 33(1)° between the two triazolopyridine rings. The centrosymmetric crystal structure is a racemic mixture, but the resolution was not possible due to a ring-chain isomerization in a solution that produces a dynamic racemization.

Caracterización mineralógica de materias primas cerámicas por métodos cuantitativos de difracción de rayos x

2002

[ES] El objetivo de este trabajo es la caracterización de fases minerales presentes en materias primas utilizadas en la industria cerámica. Para ello se utilizan dos métodos cuantitativos basados en la difracción de rayos X, el método de Rietveld y un método sin estándar. Los resultados obtenidos por difracción rayos X de estos materiales policristalinos se comparan con los correspondientes análisis químicos y la composición normativa calculada. La precisión y reproducibilidad de los resultados obtenidos, en concordancia con los del análisis químico, son una de las más importantes ventajas de la difractometría cuantitativa que facilitan su utilización en la industria cerámica en el control …

CCDC 1489441: Experimental Crystal Structure Determination

2016

Related Article: Oriol Vallcorba, Rosa Adam, Jordi Rius, Rafael Ballesteros, José M. Amigó and Belén Abarca|2014|Powder Diffr.|29|331|doi:10.1017/S0885715614000402

CCDC 1489440: Experimental Crystal Structure Determination

2016

Related Article: Oriol Vallcorba, Rosa Adam, Jordi Rius, Rafael Ballesteros, José M. Amigó and Belén Abarca|2014|Powder Diffr.|29|331|doi:10.1017/S0885715614000402