A quantitative study of vapor diffusions for crystallizations: rates and solvent parameter changes
Vapor diffusion crystallizations are among the most versatile methods for growing X-ray quality crystals. While many experimental sections describe the successful use of various solvent combinations, the literature has been entirely lacking in quantitative data (rates, measures of solvent strength c...
Saved in:
Published in | Dalton transactions : an international journal of inorganic chemistry Vol. 48; no. 3; pp. 11575 - 11582 |
---|---|
Main Authors | , , |
Format | Journal Article |
Language | English |
Published |
England
Royal Society of Chemistry
30.07.2019
|
Subjects | |
Online Access | Get full text |
Cover
Loading…
Summary: | Vapor diffusion crystallizations are among the most versatile methods for growing X-ray quality crystals. While many experimental sections describe the successful use of various solvent combinations, the literature has been entirely lacking in quantitative data (rates, measures of solvent strength changes) that might allow more informed planning rather than simple trial-and-error approaches. We here report the diffusion-induced volume changes for 44 solvent combinations over the first 60 h under standardized conditions, plus six more combinations that exhibit little or no volume changes. Additionally, the inner and outer vial compositions at 24 h were determined, and the resulting changes in solvation parameters were quantified using Hansen solubility parameters. Some general preliminary effects of changes in volume ratios and scale are described. These results identify two dozen solvent combinations with larger changes in solvent parameters than the very commonly used diethyl ether/dichloromethane example. These results should allow a more informed approach to the execution of vapor diffusion crystallizations than has previously been possible.
Quantitative data on the rates and extents of vapor diffusion for 50 solvent combinations is given to allow more informed planning of such crystallizations. |
---|---|
Bibliography: | Electronic supplementary information (ESI) available: Standard apparatus undergoing diffusion (movie), solvent properties, variable-temperature setup, and calculations of Hansen solubility parameter changes. See DOI 10.1039/c8dt01891j ObjectType-Article-1 SourceType-Scholarly Journals-1 ObjectType-Feature-2 content type line 23 |
ISSN: | 1477-9226 1477-9234 |
DOI: | 10.1039/c8dt01891j |