5OOI

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	PETRA III, EMBL c/o DESY BEAMLINE P13 (MX1)
Synchrotron site	PETRA III, EMBL c/o DESY
Beamline	P13 (MX1)
Temperature [K]	100
Detector technology	PIXEL
Collection date	2017-07-02
Detector	DECTRIS PILATUS3 6M
Wavelength(s)	1.0000
Spacegroup name	P 21 21 21
Unit cell lengths	46.488, 112.128, 143.692
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	71.480 - 1.998
R-factor	0.1748
Rwork	0.174
R-free	0.22110
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3ofm
RMSD bond length	0.011
RMSD bond angle	1.124
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]	71.480	2.070
High resolution limit [Å]	1.998	1.998
Rmerge	0.177	1.191
Number of reflections	51742	4979
<I/σ(I)>	7.39	1.41
Completeness [%]	99.7	97.59
Redundancy	6.7	6.7
CC(1/2)	0.999	0.673

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	90 MIKROLITER ENZYME STOCK SOLUTION (5 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) PEG3350, 0.2 M AMMONIUM ACETATE, 0.1 M HEPES BUFFER, PH 8.5. PRIOR TO EQUILIBRATION THE CRYSTALLIZATION DROP WAS COMPOSED OF 1 MIKROLITER RESERVOIR SOLUTION PLUS 1 MIKROLITER ENZYME/4P MIXTURE., VAPOR DIFFUSION, SITTING DROP, TEMPERATURE 293K