structural disorder and transformation in crystal growth: direct observation of ring-opening isomerization in a metal–organic solid solution

Clicks: 302
ID: 233543
2014
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Abstract
A rare example is reported in which discrete Ag2L2 ring and (AgL)∞ chain motifs [L = N,N′-bis(3-imidazol-1-yl-propyl)-pyromellitic diimide] co-crystallize in the same crystal lattice with varying ratios and degrees of disorder. Crystal structures obtained from representative crystals reveal compatible packing arrangements of the cyclic and polymeric isomers within the crystal lattice, which enables them to co-exist within a crystalline solid solution. A feasible pathway for transformation between the isomers is suggested via facile rotation of the coordinating imidazolyl groups. This chemical system could provide a chance for direct observation of ring-opening isomerization at the crystal surface. Mass spectrometry and 1H NMR titration show a dynamic equilibrium between cyclic and oligomeric species in solution, and a potential crystallization process is suggested involving alignment of precursors directed by aromatic stacking interactions between pyromellitic diimide units, followed by ring-opening isomerization at the interface between the solid and the solution. Both cyclic and oligomeric species can act as precursors, with interconversion between them being facile due to a low energy barrier for rotation of the imidazole rings. Thermogravimetric analysis and variable-temperature powder X-ray diffraction indicate a transition to a different crystalline phase around 120°C, which is associated with loss of solvent from the crystal lattice.
Reference Key
jiang2014iucrjstructural Use this key to autocite in the manuscript while using SciMatic Manuscript Manager or Thesis Manager
Authors ;Ji-Jun Jiang;Jian-Rong He;Xing-Qiang Lü;Da-Wei Wang;Guo-Bi Li;Cheng-Yong Su
Journal european journal of orthopaedic surgery & traumatology : orthopedie traumatologie
Year 2014
DOI
10.1107/S2052252514015966
URL
http://scripts.iucr.org/cgi-bin/paper?S2052252514015966
Keywords
Crystallization structural transformation solid solution

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