9QAG

Protein kinase CK2 catalytic subunit alpha' (CSNK2A2 gene product) in complex with F2X-Entry screen fragment F08 and CX-4945 (Silmitasertib)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.1
Synchrotron site	BESSY
Beamline	14.1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2024-04-18
Detector	DECTRIS PILATUS3 S 6M
Wavelength(s)	0.918400
Spacegroup name	P 1
Unit cell lengths	46.539, 47.813, 50.407
Unit cell angles	113.30, 90.04, 91.22

Refinement procedure

Resolution	32.980 - 1.010
R-factor	0.1357
Rwork	0.136
R-free	0.16170
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.012
RMSD bond angle	1.171
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER (1.20.1_4487)
Refinement software	PHENIX (1.21.2_5419)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	46.526	1.156
High resolution limit [Å]	1.007	1.007
Rmerge	0.053	0.777
Rpim	0.034	0.486
Number of reflections	175900	5226
<I/σ(I)>	5.7	1.9
Completeness [%]	49.5
Redundancy	3.2
CC(1/2)	0.999	0.507

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	Original reservoir: 900 mM LiCl, 250 mM Tris HCl, pH 8.5, 28 % PEG 6000 Protein mixture: 5 mg/mL CK2alpha Prime in 500 mM NaCl, 25 mM Tris HCl, pH 8.5, 1 mM CX-4945 and 5 % DMSO Drop: 2 microliter reservoir, 4 microliter protein/CX-4945 mix Crystal optimization by micro- and macroseeding Ligand soaking: 100 mM ligand in 900 mM LiCl, 250 mM Tris HCl, pH 8.5, 28 % PEG 6000, 5 % DMSO Equilibration for 24 h against new reservoir: 900 mM LiCl, 250 mM Tris HCl, pH 8.5, saturated PEG 6000