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Epitaxial Retrieval of a Disappearing Polymorph.


ABSTRACT: 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 ?-1, was obtained under ambient conditions. A second phase, designated ?-1, was initially also obtained by this method; however, following the advent of a third phase, ?-1, all subsequent efforts over a period of a year to crystallize ?-1 yielded either ?-1, obtained by carrying out the recrystallization at elevated temperature, or ?-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 ?-1 was an example of a "disappearing polymorph". The first phase obtained of 2, designated ?-2, was obtained by recrystallization under ambient conditions and is isomorphous and isostructural with ?-1. The second phase ?-2 was obtained by slight elevation of the recrystallization temperature and was found to be isomorphous and isostructural with ?-1. Subsequently, ?-2 was used to seed the growth of the disappearing polymorph ?-1. No third phase of 2 (?-2) has been isolated thus far.

SUBMITTER: Tidey JP 

PROVIDER: S-EPMC4291774 | biostudies-literature | 2015 Jan

REPOSITORIES: biostudies-literature

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Recrystallization of [PdCl<sub>2</sub>([9]aneS<sub>2</sub>O)] ([9]aneS<sub>2</sub>O = 1-oxa-4,7-dithiacyclononane), <b>1</b>, and [PtCl<sub>2</sub>([9]aneS<sub>2</sub>O)], <b>2</b>, by diffusion of Et<sub>2</sub>O vapor into solutions of the complexes in MeNO<sub>2</sub> yielded three phases of <b>1</b> and two phases of <b>2</b>. The known phase of <b>1</b>, herein designated α-<b>1</b>, was obtained under ambient conditions. A second phase, designated β-<b>1</b>, was initially also obtained by  ...[more]

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