7A1B

Crystal structure of human protein kinase CK2alpha' (CSNK2A2 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 ID23-2
Synchrotron site	ESRF
Beamline	ID23-2
Temperature [K]	100
Detector technology	PIXEL
Collection date	2018-11-14
Detector	DECTRIS PILATUS 2M
Wavelength(s)	0.87313
Spacegroup name	P 1
Unit cell lengths	46.256, 47.593, 50.550
Unit cell angles	113.23, 90.00, 91.13

Refinement procedure

Resolution	46.450 - 1.287
R-factor	0.158
Rwork	0.157
R-free	0.19250
Structure solution method	AB INITIO PHASING
RMSD bond length	0.007
RMSD bond angle	0.891
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	Arcimboldo
Refinement software	PHENIX (1.18.2_3874)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	46.450	1.412
High resolution limit [Å]	1.287	1.287
Rmerge	0.078	0.829
Rmeas	0.093	0.977
Rpim	0.050	0.512
Number of reflections	70878	3544
<I/σ(I)>	8.3	1.4
Completeness [%]	70.6	14.6
Redundancy	3.4	3.5
CC(1/2)	0.997	0.519

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8.5	293	Reservoir composition: 28 % (w/v) PEG6000, 0.9 M LiCl, 0.1 M, Tris/HCl, pH 8.5; drop composition prior to equilibration: 0.01 ml reservoir solution + 0.02 ml CK2alpha' (mutant Cys336Ser)/inhibitor MB002 mixture (0.180 ml 6 mg/ml CK2alpha'Cys336Ser, 0.5 M NaCl, 25 mM Tris/HCl, pH 8.5, mixed and pre-equilibrated with 0.02 ml 10 mM MB002 in dimethyl sulfoxide); the initial inhibitor MB002 was replaced by the inhibitor 5,6-dibromo-1H-triazolo[4,5-b]pyridine by extensive crystal soaking.