5EGU

FIRST DOMAIN OF HUMAN BROMODOMAIN BRD4 IN COMPLEX WITH INHIBITOR 3-Butyl-8-(6-butyl-5,7-dimethyl-[1,2,4]triazolo[1,5-a]pyrimidin-2-ylsulfanylmethyl)-7-ethyl-3,7-dihydropurine-2,6-dione

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	BRUKER AXS MICROSTAR
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2006-11-14
Detector	MAR scanner 345 mm plate
Wavelength(s)	1.541790
Spacegroup name	P 21 21 21
Unit cell lengths	69.686, 83.612, 107.391
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	45.180 - 2.210
R-factor	0.18724
Rwork	0.185
R-free	0.23530
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2oss
RMSD bond length	0.018
RMSD bond angle	1.832
Data reduction software	XDS (17 jun 2015)
Data scaling software	XDS (17 jun 2015)
Phasing software	PHASER (2.5.6)
Refinement software	REFMAC (5.8.0131)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.350
High resolution limit [Å]	2.200	2.210
Rmerge	0.104	0.480
Number of reflections	59187
<I/σ(I)>	13.15	3.44
Completeness [%]	97.8	95.2
Redundancy	4.63	4.52

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8.5	292	Ratio 1:1 (protein:precipitant). 25 mg/mL BRD4_BD1 protein. 1.0 mM inhibitor (in DMSO) final concentration. Protein buffer: 0.01M HEPES (pH 7.5), 0.15M NaCl. Precipitant agent : 0.2M Ammonium sulfate, 0.1M Tris pH 8.5, 25% PEG3350. Cryoprotectant : 10% ethylene glycol.