9R5C

Crystal structure of human protein kinase CK2 catalytic subunit (isoenzyme ck2alpha'; CSNK2A2 gene product) in complex with 4,7-dibromo-5,6-difluoro-1H-1,2,3-benzotriazole

This is a non-PDB format compatible entry.

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	2021-09-16
Detector	DECTRIS EIGER2 X CdTe 16M
Wavelength(s)	0.8856
Spacegroup name	P 1
Unit cell lengths	46.374, 47.307, 50.377
Unit cell angles	66.81, 89.93, 88.88

Refinement procedure

Resolution	32.050 - 1.040
R-factor	0.1453
Rwork	0.144
R-free	0.16390
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.017
RMSD bond angle	1.491
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]	32.050	1.127
High resolution limit [Å]	1.036	1.036
Rmerge	0.066	0.472
Number of reflections	141704	7087
<I/σ(I)>	7.6	1.6
Completeness [%]	74.1
Redundancy	3.4
CC(1/2)	0.989	0.989

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8.5	293.15	180 MICROLITER ENZYME STOCK SOLUTION (6 MG/ML IN 500 MM NACL, 25 MM TRIS/HCL, PH 8.5) WERE MIXED and incubated WITH 20 MIKROLITER of a STOCK SOLUTION of the inhibitor 4B0 (10 MM 4B0 IN DMSO). 10 MICROLITERS OF the resulting solution WERE MIXED WITH 5 MICROLITERS OF RESERVOIR SOLUTION (900 MM LICL, 28 % (W/V) PEG 6000, 100 MM TRIS/HCL, PH 8.5) IN EACH WELL OF A CRYSTALLIZATION PLATE. A SINGLE MACROSEED, grown UNDER THE SAME CONDITIONS, WAS ADDED TO EACH DROPLET of the plate. THE DROPLETS WERE EQUILIBRATED AT 293.15 K using the sitting drop variant of the VAPOR DIFFUSION method. This procedure generated large single crystals of a CK2alpha'/4B0 complex. Afterwards, the inhibitor 4B0 was exchanged against 4,7-dibromo-5,6-difluoro-1H-1,2,3-benzotriazole by an extensive soaking procedure of several steps.