5DLX

FIRST DOMAIN OF HUMAN BROMODOMAIN BRD4 IN COMPLEX WITH INHIBITOR N-{3-[4-(3-chlorophenyl)piperazin-1-yl]propyl}-1-{3-methyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl}piperidine-4-carboxamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-2
Synchrotron site	ESRF
Beamline	ID23-2
Temperature [K]	100
Detector technology	PIXEL
Collection date	2015-04-15
Detector	DECTRIS PILATUS 2M
Wavelength(s)	0.967700
Spacegroup name	P 21 21 21
Unit cell lengths	41.723, 48.509, 58.094
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	37.230 - 1.900
R-factor	0.12959
Rwork	0.125
R-free	0.20707
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2oss
RMSD bond length	0.028
RMSD bond angle	2.316
Data reduction software	XDS (jun 17, 2015)
Data scaling software	XDS (jun 17, 2015)
Phasing software	PHASER (version 2.5.6)
Refinement software	REFMAC (5.8.0131)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.020
High resolution limit [Å]	1.900	1.900
Number of reflections	9664
<I/σ(I)>	20.09	3.73
Completeness [%]	99.3	97.8
Redundancy	4.83	4.59

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	292	Ratio 1:1 (protein:precipitant). 12 mg/mL Brd4_BD1 protein. Protein buffer 10 mM HEPES (pH 7.5) 150 mM NaCl. Precipitant agent 22 % (w/v) PEG 3350, 10% (w/v) ethylene glycol 30 % (w/v), 0.3 M NaFormate. 1.0 mM inhibitor (in DMSO) final concentration. Cryoprotection with 10 % (w/v) glycerol