Hi Ana,
If this histidine is part of the active site, you may want to look into the 
catalytic mechanism to see if this histidine could react with something like a 
malonate. Active site residues can do amazing things that normal residues 
cannot. If something from your protease inhibitor cocktail would have reacted, 
this should occur in non-malonate conditions as well.

Best,
Herman

Von: CCP4 bulletin board <[email protected]> Im Auftrag von Ana Ebrecht
Gesendet: Mittwoch, 18. August 2021 13:14
An: [email protected]
Betreff: Re: [ccp4bb] malonate and histidine interaction

Hello Jon,
Thanks for the comments. Yes, the His is part of the active site, and the 
distances are very close, like a covalent bond. That's why I was wondering if 
the malonate can be bound to the His.

We tried to model the malonate in the different conformation, but that didn't 
work. But I'll check about the protease inhibitor. Thanks!

Kind regards
Ana

On Tue, 17 Aug 2021 at 14:48, Jon Cooper 
<[email protected]<mailto:[email protected]>> wrote:
Hello, only other thought was that malonate might be binding in two 
conformations, i.e. dual occupancy, and did you use a protease inhibitor 
cocktail, since the constituents can react? The density looks a bit like 
citrate, but too close to the His. I couldn't read the distances to the His in 
your figure. Is it part of the active site and if so can you say what the 
enzyme is? Anomalous difference maps are popular here, too. Is the surrounding 
structure totally OK because odd features in the difference map can indicate 
problems nearby e.g. I did see a leucine which looked slightly strained on the 
left, but maybe I am wrong. Good luck. Cheers, Jon.C.


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-------- Original Message --------
On 17 Aug 2021, 12:11, Ana Ebrecht < 
[email protected]<mailto:[email protected]>> wrote:

Hi Jon,
Thanks for the reply. I don't think this is acetylation, because I only see 
this density in the crystals that grew with malonate. In other conditions 
doesn't show anything like that. So I thought it'd be the malonate. But I'll 
check on that.
Thanks for the suggestion.

Kind regards
Ana

On Mon, 16 Aug 2021 at 16:56, Jon Cooper 
<[email protected]<mailto:[email protected]>> wrote:
Hello, could the His be partially acetylated?

Best wishes Jon.C.


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-------- Original Message --------
On 16 Aug 2021, 14:52, Ana Ebrecht < 
[email protected]<mailto:[email protected]>> wrote:

Dear all,

I am building the structure of a protein that was crystallized in 0.2 M sodium 
malonate pH 5.0, 20% w/v polyethylene glycol 3,350.
During the refinement, we found what we think is a malonate molecule in the 
active site, but it seems like is bound somehow to the histidine (this His is 
the catalytic residue of the enzyme), almost like a covalent interaction. Under 
other conditions of crystallization, the protein bound a sulfate and an acetate 
in the site but did not show this type of interaction with the histidine.

We couldn't find anything that explains a reaction between the malonate and the 
histidine.
Does anyone have experience with this reaction or have seen something similar 
before?

Thanks
Kind regards
Ana





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