5ONI

LOW-SALT STRUCTURE OF PROTEIN KINASE CK2 CATALYTIC SUBUNIT (ISOFORM CK2ALPHA) IN COMPLEX WITH THE INDENOINDOLE-TYPE INHIBITOR 4P

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE MASSIF-1
Synchrotron site	ESRF
Beamline	MASSIF-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2016-12-15
Detector	DECTRIS PILATUS 2M
Wavelength(s)	0.9660
Spacegroup name	P 43 21 2
Unit cell lengths	128.453, 128.453, 124.106
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	57.041 - 2.000
R-factor	0.1757
Rwork	0.175
R-free	0.20420
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2pvr
RMSD bond length	0.007
RMSD bond angle	0.807
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	PHENIX ((1.12_2829: ???))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	57.041	2.072
High resolution limit [Å]	2.000	2.000
Rmerge	0.065	1.909
Number of reflections	70221	6881
<I/σ(I)>	14.2	0.93
Completeness [%]	99.5	98.84
Redundancy	6.2	6.3
CC(1/2)	0.999	0.437

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	90 MICROLITER ENZYME STOCK SOLUTION (6 MG/ML IN 500 MM NACL, 25 MM TRIS/HCL, PH 8.5) WAS MIXED WITH 10 MIKROLITER 4P STOCK SOLUTION (10 MM 4P IN DMSO). THIS MIXTURE WAS INCUBATED FOR 30 MIN AT ROOM TEMPERATURE. THE RESERVOIR SOLUTION OF THE CRYSTALLIZATION EXPERIMENT WAS 25 % (W/V) PEG5000, 0.2 M AMMONIUM SULPHATE, 0.1 M MES BUFFER, PH 6.5. PRIOR TO EQUILIBRATION THE CRYSTALLIZATION DROP WAS COMPOSED OF 1 MICROLITER RESERVOIR SOLUTION PLUS 1 MICROLITER ENZYME/4P MIXTURE., VAPOR DIFFUSION, SITTING DROP, TEMPERATURE 293K