7Q6W

Crystal structure of the bromodomain of ATAD2 with triazolopyridazine (cpd 22)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E+
Temperature [K]	100
Detector technology	CCD
Collection date	2015-07-07
Detector	RIGAKU SATURN 944+
Wavelength(s)	1.5406
Spacegroup name	P 65 2 2
Unit cell lengths	79.291, 79.291, 138.014
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	48.680 - 1.960
R-factor	0.1914
Rwork	0.190
R-free	0.21030
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	internal model
RMSD bond length	0.010
RMSD bond angle	0.890
Data scaling software	Aimless (0.5.9)
Phasing software	AMoRE
Refinement software	BUSTER (2.11.6)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	48.680	48.680	2.060
High resolution limit [Å]	1.960	6.190	1.960
Rmerge	0.053	0.019	0.405
Rmeas	0.060	0.021	0.507
Rpim	0.026	0.010	0.299
Total number of observations	85891	3349	6404
Number of reflections	17803	713	2586
<I/σ(I)>	22.3	67.6	2.6
Completeness [%]	92.4	99.4	95.4
Redundancy	4.8	4.7	2.5
CC(1/2)	0.999	0.999	0.751

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	6.25	293	ATAD2 (981-1108) at 12 mg/ml in 25 mM Tris pH 9.7, 300 mM NaCl, 0.5 mM TCEP crystallised from 20% PEG 3350, 0.2 M ammonium sulfate, 0.1 M Bis-Tris pH 6.25. Ligands were introduced by soaking, cryo-protection with 20 % glycerol.