5V67

CRYSTAL STRUCTURE OF THE FIRST BROMODOMAIN OF HUMAN BRD4 IN COMPLEX WITH Volasertib

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 22-ID
Synchrotron site	APS
Beamline	22-ID
Temperature [K]	100
Detector technology	CCD
Collection date	2014-04-20
Detector	MARMOSAIC 300 mm CCD
Wavelength(s)	1.00
Spacegroup name	P 21 21 21
Unit cell lengths	38.240, 42.210, 93.440
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	38.467 - 1.780
R-factor	0.1532
Rwork	0.150
R-free	0.20770
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4o70
RMSD bond length	0.010
RMSD bond angle	1.286
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (1.9_1692)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	38.467	38.467	1.830
High resolution limit [Å]	1.780	7.960	1.780
Rmerge	0.065	0.032	0.333
Rmeas	0.070	0.036	0.359
Number of reflections	15100	204	1106
<I/σ(I)>	21.18	43.14	5.92
Completeness [%]	100.0	99	100
Redundancy	7.165	5.77	7.235
CC(1/2)	0.999	0.999	0.966

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	291	12.5 MG/ML BRD4, 5MM HEPES PH 7.5, 50MM SODIUM CHLORIDE, 0.5MM DTT, 50MM TRIS PH8.5, 0.1M AMMONIUM, SULFATE, 12.5% PEG 3,350, 10% DMSO, 1 MM Volasertib