Hi Nian,

This isn't a solution but I remember seeing an excellent talk by Annie
Hassell at the CCP4 study weekend a couple of years back.

The paper from that talk may help you out.


Acta Cryst. (2007). D63, 72-79  [ doi:10.1107/S0907444906047020 ]
Crystallization of protein-ligand complexes
A. M. Hassell, G. An, R. K. Bledsoe, J. M. Bynum, H. L. Carter,
S.-J.J. Deng, R. T. Gampe, T. E. Grisard, K. P. Madauss, R. T. Nolte,
W. J. Rocque, L. Wang, K. L. Weaver, S. P. Williams, G. B. Wisely, R.
Xu and L. M. Shewchuk

Synopsis: Methods presented for growing protein-ligand complexes fall
into the categories of co-expression of the protein with the ligands
of interest, use of the ligands during protein purification,
cocrystallization and soaking the ligands into existing crystals.


HTH,

Dave


On 12/09/2007, Joe Krahn <[EMAIL PROTECTED]> wrote:
> I am working with a protein/ligand complex that is very resistant. to
> getting a stable complex. The first thing to try is to go to saturating
> ligand concentrations, even if it seems that it is excessive. It is
> possible that binding affinity is significantly different.
>
> My biggest problem is precipitant interfering with binding, combined
> with relatively low substrate solubility. I tried transferring to a
> different condition, but it seems that most precipitating agents have a
> solubility affect on the ligand as well. I ended up screening conditions
> just to understand ligand solubilities. I even tried things like DMSO
> additives.
>
> Eventually, I found conditions where the ligand is fairly soluble, but
> also stabilizes the protein. I found that ethylene glycol helped binding
> even though glycerol inhibited it. I also changed the pH, and did the
> soak at room temperature instead of in the cold room. Even then, I used
> saturating ligand concentrations.
>
> Joe Krahn
>
> Nian Huang wrote:
> > Dear All,
> >
> > I have been trying to get a protein-ligand complex crystal for a long
> > time. Here, ligand is either substrate or product for this kinase. I
> > have tried many methods: soaking with apo-crystal, co-crystal with
> > different concentration of ligand and screen for new conditions. I got
> > a couple of co-crystals with the new conditions, but still no ligand
> > was found in the active site.
> >
> > Anybody has some new ideas that I can try? I have been using glycerol
> > as my cryoprotectant. Could cryoprotectant have some negative effect
> > on co-crystal? I will try to collect some data at room temperature in
> > the future.
> >
> > Thank you in advance for your suggestion.
> >
> > Nian
> >
> > Dept of Biochemistry
> > UT Southwestern Medical Center
>



-- 
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David Briggs, PhD.
Father & Crystallographer
www.dbriggs.talktalk.net
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