7A4B

Crystal structure of human protein kinase CK2alpha (CSNK2A1 gene product) in complex with the ATP-competitive inhibitor 5,6-dibromo-1H-triazolo[4,5-b]pyridine

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID29
Synchrotron site	ESRF
Beamline	ID29
Temperature [K]	100
Detector technology	PIXEL
Collection date	2016-12-13
Detector	DECTRIS PILATUS 6M-F
Wavelength(s)	0.976251
Spacegroup name	P 43 21 2
Unit cell lengths	127.329, 127.329, 124.884
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	90.035 - 2.060
R-factor	0.192
Rwork	0.191
R-free	0.22260
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2pvr
RMSD bond length	0.001
RMSD bond angle	0.402
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	PHENIX (1.18.2_3874)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	90.035	2.260
High resolution limit [Å]	2.060	2.060
Rmerge	0.178	2.105
Rmeas	0.181	2.166
Rpim	0.036	0.492
Number of reflections	46838	2341
<I/σ(I)>	14.8	1.6
Completeness [%]	73.3	15.3
Redundancy	25.7	18.1
CC(1/2)	0.997	0.483

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293.15	1 MIKROLITER OF THE CK2ALPHA/INHIBITOR MIXTURE (COMPOSITION: 7 MG/ML CK2ALPHA ENZYME, 1 MILLIMOLAR INHIBITOR, 10 % DIMETHYL SULFOXIDE, 450 MM NACL, 22.5 MM TRIS/HCL, PH 8.5) WAS MIXED WITH 1 MIKROLITER RESERVOIR SOLUTION (COMPOSITION: 25 % PEG3350, 0.2 M AMMONIUM SULPHATE, 0.1 M BIS-TRIS BUFFER, PH 5.5) FOLLOWED BY VAPOUR DIFFUSION EQUILIBRATION AGAINST THE RESERVOIR SOLUTION.