5M4C

Complex structure of human protein kinase CK2 catalytic subunit with a thieno[2,3-d]pyrimidin inhibitor crystallized under low-salt conditions

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X06DA
Synchrotron site	SLS
Beamline	X06DA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-10-20
Detector	DECTRIS PILATUS 2M
Wavelength(s)	1.0000
Spacegroup name	P 21 21 21
Unit cell lengths	48.104, 79.418, 82.341
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	41.535 - 1.935
R-factor	0.1584
Rwork	0.157
R-free	0.19680
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2pvr
RMSD bond length	0.009
RMSD bond angle	1.031
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHENIX
Refinement software	PHENIX ((1.10.1_2155: ???))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	41.600	2.004
High resolution limit [Å]	1.935	1.935
Rmerge	0.098	0.731
Number of reflections	23281
<I/σ(I)>	15.25	2.26
Completeness [%]	96.0	62
Redundancy	6.3	5.2
CC(1/2)	0.998	0.758

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	PROTEIN STOCK SOLUTION: 6 MG/M CK2ALPHA1-335 IN 0.5 M NACL, 25 MM TRIS/HCL, PH 8.5; INHIBITOR STOCK SOLUTION: 10 MM INHIBITOR IN DMSO; PROTEIN/INHIBITOR COMPLEX SOLUTION: 90 MICROLITER PROTEIN STOCK SOLUTION + 10 MICROLITER INHIBITOR STOCK SOLUTION; RESERVOIR SOLUTION: 24 % (w/v) PEG8000, 0.2 M KCl; DROP SOLUTION BEFORE EQULIBRATION: 0.3 MICROLITER PROTEIN/INHIBITOR COMPLEX SOLUTION + 0.3 MICROLITER RESERVOIR SOLUTION