Home >
Community >
How to recrystallize complexes from the solvent pair acetone/water?
Upvote
21
Downvote
+ Inorganic chemistry
+ Solvents
+ Chemistry
Posted by
Khaled Ahmed
How to recrystallize complexes from the solvent pair acetone/water?
Please check solubility of your compounds in common organic solvents; both polar and non-polar. Select two solvents in which your compounds are i) highly soluble and, ii) least soluble, but both the solvents should be miscible with each other. Dissolve your compound in a small quantity of solvent in which it is highly soluble. To this solution, add drop-wise the other solvent until you see turbidity, stop at this stage, and add a few more drops of first solvent to get a clear solution. Store it at zero deg C, undisturbed for a day or two. I am sure you get X-ray quality crystals. This is the usual practice to crystallize most of the solid compounds with moderate solubility in organic solvents.
dichloromethane-hexane, dichloroethane-hexane or pentane are ideal combinations.
Please check solubility of your compounds in common organic solvents; both polar and non-polar. Select two solvents in which your compounds are i) highly soluble and, ii) least soluble, but both the solvents should be miscible with each other. Dissolve your compound in a small quantity of solvent in which it is highly soluble. To this solution, add drop-wise the other solvent until you see turbidity, stop at this stage, and add a few more drops of first solvent to get a clear solution. Store it at zero deg C, undisturbed for a day or two. I am sure you get X-ray quality crystals. This is the usual practice to crystallize most of the solid compounds with moderate solubility in organic solvents.
dichloromethane-hexane, dichloroethane-hexane or pentane are ideal combinations.
Dear Cheng Yun Wu many thanks for sharing this very interesting technical question with the RG community. It might be worth a try using acetonitrile to recrystallize your ionic ruthenium complexes. Often such compounds show a good solubilty in hot acetonitrile and form nice crystals upon cooling of the solution to room temperature. Hot water alone might also be worth a try. If your compounds are very soluble in acetone, you could also try a vapor diffusion technique in which you let diethyl ether diffuse into the actone solution. For more potentially useful suggestions please also have a look at the attached guides to growing single crystals. Good luck with your experiments and best wishes, Frank Edelmann
Dear Cheng Yun Wu many thanks for sharing this very interesting technical question with the RG community. It might be worth a try using acetonitrile to recrystallize your ionic ruthenium complexes. Often such compounds show a good solubilty in hot acetonitrile and form nice crystals upon cooling of the solution to room temperature. Hot water alone might also be worth a try. If your compounds are very soluble in acetone, you could also try a vapor diffusion technique in which you let diethyl ether diffuse into the actone solution. For more potentially useful suggestions please also have a look at the attached guides to growing single crystals. Good luck with your experiments and best wishes, Frank Edelmann
Dear Cheng Yun Wu many thanks for sharing this very interesting technical question with the RG community. It might be worth a try using acetonitrile to recrystallize your ionic ruthenium complexes. Often such compounds show a good solubilty in hot acetonitrile and form nice crystals upon cooling of the solution to room temperature. Hot water alone might also be worth a try. If your compounds are very soluble in acetone, you could also try a vapor diffusion technique in which you let diethyl ether diffuse into the actone solution. For more potentially useful suggestions please also have a look at the attached guides to growing single crystals. Good luck with your experiments and best wishes, Frank Edelmann
Dear Cheng Yun Wu many thanks for sharing this very interesting technical question with the RG community. It might be worth a try using acetonitrile to recrystallize your ionic ruthenium complexes. Often such compounds show a good solubilty in hot acetonitrile and form nice crystals upon cooling of the solution to room temperature. Hot water alone might also be worth a try. If your compounds are very soluble in acetone, you could also try a vapor diffusion technique in which you let diethyl ether diffuse into the actone solution. For more potentially useful suggestions please also have a look at the attached guides to growing single crystals. Good luck with your experiments and best wishes, Frank Edelmann
One factor I don't think has been mentioned so far is that solvent can inherently influence crystal nucleation and growth by virtue of the solvent - crystal surface interactions. This is most often observed as an impact on the final morphology. So trying a range of solvents is well worth it, by evaporation, diffusion, and cooling. Trace impurities that are surface active can also have.a profound impact on crystal growth, so ensuring your sample is as pure as possible can be very important in some systems.
One factor I don't think has been mentioned so far is that solvent can inherently influence crystal nucleation and growth by virtue of the solvent - crystal surface interactions. This is most often observed as an impact on the final morphology. So trying a range of solvents is well worth it, by evaporation, diffusion, and cooling. Trace impurities that are surface active can also have.a profound impact on crystal growth, so ensuring your sample is as pure as possible can be very important in some systems.
Please check solubility of your compounds in common organic solvents; both polar and non-polar. Select two solvents in which your compounds are i) highly soluble and, ii) least soluble, but both the solvents should be miscible with each other. Dissolve your compound in a small quantity of solvent in which it is highly soluble. To this solution, add drop-wise the other solvent until you see turbidity, stop at this stage, and add a few more drops of first solvent to get a clear solution. Store it at zero deg C, undisturbed for a day or two. I am sure you get X-ray quality crystals. This is the usual practice to crystallize most of the solid compounds with moderate solubility in organic solvents.
dichloromethane-hexane,
dichloroethane-hexane or pentane are ideal combinations.
All the best
Balakrishna
Please check solubility of your compounds in common organic solvents; both polar and non-polar. Select two solvents in which your compounds are i) highly soluble and, ii) least soluble, but both the solvents should be miscible with each other. Dissolve your compound in a small quantity of solvent in which it is highly soluble. To this solution, add drop-wise the other solvent until you see turbidity, stop at this stage, and add a few more drops of first solvent to get a clear solution. Store it at zero deg C, undisturbed for a day or two. I am sure you get X-ray quality crystals. This is the usual practice to crystallize most of the solid compounds with moderate solubility in organic solvents.
dichloromethane-hexane,
dichloroethane-hexane or pentane are ideal combinations.
All the best
Balakrishna
More
VOTE
Dear Cheng Yun Wu many thanks for sharing this very interesting technical question with the RG community. It might be worth a try using acetonitrile to recrystallize your ionic ruthenium complexes. Often such compounds show a good solubilty in hot acetonitrile and form nice crystals upon cooling of the solution to room temperature. Hot water alone might also be worth a try. If your compounds are very soluble in acetone, you could also try a vapor diffusion technique in which you let diethyl ether diffuse into the actone solution. For more potentially useful suggestions please also have a look at the attached guides to growing single crystals.
Good luck with your experiments and best wishes, Frank Edelmann
Dear Cheng Yun Wu many thanks for sharing this very interesting technical question with the RG community. It might be worth a try using acetonitrile to recrystallize your ionic ruthenium complexes. Often such compounds show a good solubilty in hot acetonitrile and form nice crystals upon cooling of the solution to room temperature. Hot water alone might also be worth a try. If your compounds are very soluble in acetone, you could also try a vapor diffusion technique in which you let diethyl ether diffuse into the actone solution. For more potentially useful suggestions please also have a look at the attached guides to growing single crystals.
Good luck with your experiments and best wishes, Frank Edelmann
More
VOTE
Dear Cheng Yun Wu many thanks for sharing this very interesting technical question with the RG community. It might be worth a try using acetonitrile to recrystallize your ionic ruthenium complexes. Often such compounds show a good solubilty in hot acetonitrile and form nice crystals upon cooling of the solution to room temperature. Hot water alone might also be worth a try. If your compounds are very soluble in acetone, you could also try a vapor diffusion technique in which you let diethyl ether diffuse into the actone solution. For more potentially useful suggestions please also have a look at the attached guides to growing single crystals.
Good luck with your experiments and best wishes, Frank Edelmann
Dear Cheng Yun Wu many thanks for sharing this very interesting technical question with the RG community. It might be worth a try using acetonitrile to recrystallize your ionic ruthenium complexes. Often such compounds show a good solubilty in hot acetonitrile and form nice crystals upon cooling of the solution to room temperature. Hot water alone might also be worth a try. If your compounds are very soluble in acetone, you could also try a vapor diffusion technique in which you let diethyl ether diffuse into the actone solution. For more potentially useful suggestions please also have a look at the attached guides to growing single crystals.
Good luck with your experiments and best wishes, Frank Edelmann
More
VOTE
One factor I don't think has been mentioned so far is that solvent can inherently influence crystal nucleation and growth by virtue of the solvent - crystal surface interactions. This is most often observed as an impact on the final morphology. So trying a range of solvents is well worth it, by evaporation, diffusion, and cooling. Trace impurities that are surface active can also have.a profound impact on crystal growth, so ensuring your sample is as pure as possible can be very important in some systems.
One factor I don't think has been mentioned so far is that solvent can inherently influence crystal nucleation and growth by virtue of the solvent - crystal surface interactions. This is most often observed as an impact on the final morphology. So trying a range of solvents is well worth it, by evaporation, diffusion, and cooling. Trace impurities that are surface active can also have.a profound impact on crystal growth, so ensuring your sample is as pure as possible can be very important in some systems.
More
VOTE