Epitaxial Retrieval of a Disappearing Polymorph
| Autor: | Alexander Markevich, Henry L. S. Wong, Elena Bichoutskaia, Martin Schröder, Alexander J. Blake, Jonathan McMaster, Geoffrey A. Lawrance, Jeremiah P. Tidey, Alice E. O'Connor, Joseph J. P. Cavan |
|---|---|
| Rok vydání: | 2014 |
| Předmět: |
Materials science
Recrystallization (metallurgy) Nanotechnology 02 engineering and technology General Chemistry 010402 general chemistry 021001 nanoscience & nanotechnology Condensed Matter Physics Epitaxy 01 natural sciences Article 0104 chemical sciences Crystallography Third phase General Materials Science Isostructural 0210 nano-technology |
| Zdroj: | Crystal Growth & Design |
| ISSN: | 1528-7505 1528-7483 |
| DOI: | 10.1021/cg500967w |
| Popis: | Recrystallization of [PdCl2([9]aneS2O)] ([9]aneS2O = 1-oxa-4,7-dithiacyclononane), 1, and [PtCl2([9]aneS2O)], 2, by diffusion of Et2O vapor into solutions of the complexes in MeNO2 yielded three phases of 1 and two phases of 2. The known phase of 1, herein designated α-1, was obtained under ambient conditions. A second phase, designated β-1, was initially also obtained by this method; however, following the advent of a third phase, γ-1, all subsequent efforts over a period of a year to crystallize β-1 yielded either γ-1, obtained by carrying out the recrystallization at elevated temperature, or α-1, commonly found throughout the study. This persistent absence of a phase which could initially be crystallized with ease led us to the conclusion that β-1 was an example of a “disappearing polymorph”. The first phase obtained of 2, designated α-2, was obtained by recrystallization under ambient conditions and is isomorphous and isostructural with α-1. The second phase β-2 was obtained by slight elevation of the recrystallization temperature and was found to be isomorphous and isostructural with β-1. Subsequently, β-2 was used to seed the growth of the disappearing polymorph β-1. No third phase of 2 (γ-2) has been isolated thus far. Following the discovery of a third polymorph of [PdCl2([9]aneS2O)] ([9]aneS2O = 1-oxa-4,7-dithiacyclononane), the second polymorph could no longer be grown and was therefore designated as a “disappearing polymorph”. The subsequent discovery that a closely analogous Pt(II) complex [PtCl2([9]aneS2O)] formed an isomorphous phase allowed the recovery of the lost polymorph by means of epitaxy. |
| Databáze: | OpenAIRE |
| Externí odkaz: |
|