5M44

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

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU MICROMAX-007 HF
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2012-01-20
Detector	MARRESEARCH
Wavelength(s)	1.54179
Spacegroup name	P 43 21 2
Unit cell lengths	72.061, 72.061, 131.579
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	27.841 - 2.710
R-factor	0.2225
Rwork	0.219
R-free	0.25930
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3nsz
RMSD bond length	0.003
RMSD bond angle	0.535
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]	28.000	2.807
High resolution limit [Å]	2.710	2.710
Rmerge	0.131	0.808
Number of reflections	9935
<I/σ(I)>	15.75	2.32
Completeness [%]	100.0	98
Redundancy	6.9	5.9
CC(1/2)	0.996	0.693

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5	293	Protein stock solution: 6 mg/ml 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: 4.2 M NaCl, 0.1 M sodium citrate, pH 5.0; Drop solution before equlibration: 0.5 microliter protein/inhibitor complex solution + 0.5 microliter reservoir solution