Please see:

Dym, O., Song, W., Felder, C., Roth, E., Shnyrov, V., Ashani, Y., Xu, Y., 
Joosten, R. P., Weiner, L., Sussman, J. L. & Silman, I. The impact of 
crystallization conditions on structure-based drug design: A case study on the 
methylene blue/acetylcholinesterase complex. Protein Sci. 25, 1096-1114 (2016).


Structure-based drug design utilizes apoprotein or complex structures retrieved 
from the PDB. >57% of crystallographic PDB entries were obtained with 
polyethylene glycols (PEGs) as precipitant and/or as cryoprotectant, but <6% of 
these report presence of individual ethyleneglycol oligomers. We report a case 
in which ethyleneglycol oligomers' presence in a crystal structure markedly 
affected the bound ligand's position. Specifically, we compared the positions 
of methylene blue and decamethonium in acetylcholinesterase complexes obtained 
using isomorphous crystals precipitated with PEG200 or ammonium sulfate. The 
ligands' positions within the active-site gorge in complexes obtained using 
PEG200 are influenced by presence of ethyleneglycol oligomers in both cases 
bound to W84 at the gorge's bottom, preventing interaction of the ligand's 
proximal quaternary group with its indole. Consequently, both ligands are ∼3.0Å 
further up the gorge than in complexes obtained using crystals precipitated 
with ammonium sulfate, in which the quaternary groups make direct π-cation 
interactions with the indole. These findings have implications for 
structure-based drug design, since data for ligand-protein complexes with 
polyethylene glycol as precipitant may not reflect the ligand's position in its 
absence, and could result in selecting incorrect drug discovery leads. Docking 
methylene blue into the structure obtained with PEG200, but omitting the 
ethyleneglycols, yields results agreeing poorly with the crystal structure; 
excellent agreement is obtained if they are included. Many proteins display 
features in which precipitants might lodge. It will be important to investigate 
presence of precipitants in published crystal structures, and whether it has 
resulted in misinterpreting electron density maps, adversely affecting drug 
design.

and the cover image showing the PEG molecules, in blue with their surrounding 
electron density, near the bound ligand,  methylene blue, in pink.

best regards
Joel
[cid:[email protected]]

--------------------------------------------------------------------------------
Prof. Joel L. Sussman                              
[email protected]<mailto:[email protected]>   
www.weizmann.ac.il/~joel<http://www.weizmann.ac.il/~joel>
Dept. of Structural Biology   tel: +972  (8) 934 6309  
proteopedia.org<http://www.weizmann.ac.il/~joel>
Weizmann Institute of Science fax: +972  (8) 934 6312
Rehovot 76100 ISRAEL          mob: +972 (50) 510 9600
---------------------------------------------------------------------------------

On 2Apr, 2019, at 4:12, Zhen Luo 
<[email protected]<mailto:[email protected]>> wrote:

Hi everyone,

Thank you very much for your help and time. A PEG fragment indeed seems to fit 
into the density. Thanks again!
<image001.png>

Best regards,
Zhen
From: CCP4 bulletin board <[email protected]<mailto:[email protected]>> 
on behalf of Zhen Luo <[email protected]<mailto:[email protected]>>
Reply-To: Zhen Luo <[email protected]<mailto:[email protected]>>
Date: Tuesday, 2 April 2019 at 9:01 AM
To: "[email protected]<mailto:[email protected]>" 
<[email protected]<mailto:[email protected]>>
Subject: [ccp4bb] unidentified crescent-shaped electron density

Dear all,

Could you please shed some light on what this crescent-shaped density around 
the lysine side chain might belong to? I now have two unrelated protein 
structures where this kind of density can be found surrounding a lysine side 
chain.

<image002.png><image003.png>

<image004.png><image005.png>
2FOFC maps were contoured at around 1.5 sigma, FOFC map at 3 sigma.


One protein was crystallised in 0.1 M CaCl2 and 20% PEG 3350; the other in 10% 
PEG 20000, 20% PEG MME 550, 0.03 M CaCl2/MgCl2, 0.1 M MES/imidazole. Protein 
buffers contained 0.025 M HEPES and 0.15 M NaCl. None of these fitted in well. 
Could it be cleaved PEG?

Any suggestion would be greatly appreciated. Thanks in advance!

Best regards,
Zhen Luo

School of Chemistry and Molecular Biosciences
The University of Queensland, Australia


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