Synthesis and crystal structures of two novel triazolopyridine compounds solved by local L.S. minimizations from powder diffraction data
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…
Application of delta recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes
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…
Synthesis and structural properties of hexaaza[5]helicene containing two [1,2,3]triazolo[1,5-a]pyridine moieties
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.
CCDC 1489441: Experimental Crystal Structure Determination
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
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