9R57

Crystal structure of human protein kinase CK2 catalytic subunit (isoenzyme ck2alpha'; CSNK2A2 gene product) in complex with 5,6-dibromo-1H-1,2,3-benzotriazole

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-1
Synchrotron site	ESRF
Beamline	ID23-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2022-04-22
Detector	DECTRIS EIGER2 X CdTe 16M
Wavelength(s)	0.8856
Spacegroup name	P 1
Unit cell lengths	46.109, 47.423, 50.453
Unit cell angles	113.19, 90.23, 91.30

Refinement procedure

Resolution	23.630 - 1.100
R-factor	0.1311
Rwork	0.130
R-free	0.15000
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.019
RMSD bond angle	1.433
Data reduction software	autoPROC
Data scaling software	autoPROC
Phasing software	PHASER
Refinement software	PHENIX (1.21.2_5419)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	46.371	1.156
High resolution limit [Å]	1.095	1.095
Rmerge	0.067	0.526
Number of reflections	129390	6470
<I/σ(I)>	4.4	1.6
Completeness [%]	80.0
Redundancy	2.2
CC(1/2)	0.990	0.533

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	Reservoir: 900 mM LiCl, 100 mM TRIS-HCl pH 8.5, 28 % PEG6000 Inititial drop: 5 mg per mL CK2alpha Prime with 1 mM MB002, 10 percent DMSO mixed in 2:1 ratio with reservoir (10 and 5 microliter). Optimization of crystal by microseeding and macroseeding. Complex formation by extensive purging with reservoir solution and extensive soaking at compounds saturation limit.