Carbon dioxide as a solubility "switch" for the reversible dissolution of highly fluorinated complexes and reagents in organic solvents: application to crystallization.
Highly fluorinated organic or organometallic solid compounds can be made to dissolve in liquid hydrocarbons by the application of 20-70 bar of CO(2) gas. Subsequently releasing the gas causes the compounds to precipitate or crystallize, giving quantitative recovery of the solid. The resulting crystals can be of sufficient quality for single-crystal X-ray crystallography; the structures of Rh(2)(O(2)CCF(2)CF(2)CF(3))(4)(DMF)(2), Rh(2)(O(2)C(CF(2))(9)F)(4)(MeOH)(2), Cr(hfacac)(3), and P[C(6)H(3)(3,5-CF(3))(2)](3) have been determined from crystals grown in this manner.
Jessop
Philip G
PG
Department of Chemistry, University of California, Davis, California 95616-5295, USA. jessop@chem.ucdavis.edu
Olmstead
Marilyn M
MM
Ablan
Christopher D
CD
Grabenauer
Megan
M
Sheppard
Daniel
D
Eckert
Charles A
CA
Liotta
Charles L
CL