6HBN

HIGH-SALT STRUCTURE OF PROTEIN KINASE CK2 CATALYTIC SUBUNIT (ISOFORM CK2ALPHA/CSKN2A1 GENE PRODUCT) IN COMPLEX WITH THE INDENOINDOLE-TYPE INHIBITOR THN27

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID30B
Synchrotron site	ESRF
Beamline	ID30B
Temperature [K]	100
Detector technology	PIXEL
Collection date	2017-02-04
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.976250
Spacegroup name	P 21 21 21
Unit cell lengths	71.550, 71.620, 128.030
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	64.015 - 1.590
R-factor	0.1876
Rwork	0.187
R-free	0.21720
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	5cqu
RMSD bond length	0.006
RMSD bond angle	0.806
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX ((1.13_2998: ???))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	64.016	1.647
High resolution limit [Å]	1.590	1.590
Rmerge	0.088	1.361
Rmeas	0.097	1.493
Rpim	0.039	0.607
Number of reflections	88883	8769
<I/σ(I)>	10.2	1.02
Completeness [%]	99.8	99.83
Redundancy	6.2	5.9
CC(1/2)	0.998	0.835

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.5	293.15	90 MIKROLITER ENZYME STOCK SOLUTION (6 MG/ML IN 500 MM NACL, 25 MM TRIS/HCL, PH 8.5) WAS MIXED WITH 10 MIKROLITER INHIBITOR STOCK SOLUTION (10 MM INHIBITOR IN DMSO). THIS MIXTURE WAS INCUBATED FOR 30 MIN AT ROOM TEMPERATURE. THE RESERVOIR SOLUTION OF THE CRYSTALLIZATION EXPERIMENT WAS 4.4 M NACL, 0.1 M CITRIC ACID, PH 5.5. PRIOR TO EQUILIBRATION THE CRYSTALLIZATION DROP WAS COMPOSED OF 1 MIKROLITER RESERVOIR SOLUTION PLUS 1 MIKROLITER ENZYME/INHIBITOR MIXTURE.,VAPOR DIFFUSION, SITTING DROP, TEMPERATURE 293.15K