Epitaxial Retrieval of a Disappearing Polymorph

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• 作者：Jeremiah P. Tidey ; Alice E. O鈥機onnor ; Alexander Markevich ; Elena Bichoutskaia ; Joseph J. P. Cavan ; Geoffrey A. Lawrance ; Henry L. S. Wong ; Jonathan McMaster ; Martin Schr枚der ; Alexander J. Blake
• 刊名：Crystal Growth & Design
• 出版年：2015
• 出版时间：January 7, 2015
• 年：2015
• 卷：15
• 期：1
• 页码：115-123
• 全文大小：422K
• ISSN：1528-7505

文摘

Recrystallization of [PdClb>2b>([9]aneSb>2b>O)] ([9]aneSb>2b>O = 1-oxa-4,7-dithiacyclononane), <b>1b>, and [PtClb>2b>([9]aneSb>2b>O)], <b>2b>, by diffusion of Etb>2b>O vapor into solutions of the complexes in MeNOb>2b> yielded three phases of <b>1b> and two phases of <b>2b>. The known phase of <b>1b>, herein designated 伪-<b>1b>, was obtained under ambient conditions. A second phase, designated 尾-<b>1b>, was initially also obtained by this method; however, following the advent of a third phase, 纬-<b>1b>, all subsequent efforts over a period of a year to crystallize 尾-<b>1b> yielded either 纬-<b>1b>, obtained by carrying out the recrystallization at elevated temperature, or 伪-<b>1b>, commonly found throughout the study. This persistent absence of a phase which could initially be crystallized with ease led us to the conclusion that 尾-<b>1b> was an example of a 鈥渄isappearing polymorph鈥? The first phase obtained of <b>2b>, designated 伪-<b>2b>, was obtained by recrystallization under ambient conditions and is isomorphous and isostructural with 伪-<b>1b>. The second phase 尾-<b>2b> was obtained by slight elevation of the recrystallization temperature and was found to be isomorphous and isostructural with 尾-<b>1b>. Subsequently, 尾-<b>2b> was used to seed the growth of the disappearing polymorph 尾-<b>1b>. No third phase of <b>2b> (纬-<b>2b>) has been isolated thus far.