9Q9D

Protein kinase CK2 catalytic subunit alpha' (CSNK2A2 gene product) in complex with F2X-Entry screen fragment D06 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	46.513, 47.804, 50.522
Unit cell angles	113.44, 90.11, 91.25

Refinement procedure

Resolution	32.640 - 0.890
R-factor	0.1482
Rwork	0.148
R-free	0.15850
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.013
RMSD bond angle	1.238
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	PHENIX (1.21.2_5419)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	46.350	1.026
High resolution limit [Å]	0.890	0.890
Rmerge	1.206	1.224
Rpim	0.616	0.656
Number of reflections	183402	9170
<I/σ(I)>	10.1	1.8
Completeness [%]	60.3
Redundancy	5.9
CC(1/2)	0.997	0.345

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