5M56

Monoclinic complex structure of human protein kinase CK2 catalytic subunit (isoform CK2alpha') with the inhibitor 4'-carboxy-6,8-chloro-flavonol (FLC21)

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 PILATUS3 2M
Wavelength(s)	1.00000
Spacegroup name	P 1 21 1
Unit cell lengths	69.341, 87.620, 72.977
Unit cell angles	90.00, 109.69, 90.00

Refinement procedure

Resolution	43.810 - 2.237
R-factor	0.1648
Rwork	0.164
R-free	0.20630
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3ofm
RMSD bond length	0.002
RMSD bond angle	0.516
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]	44.000	2.317
High resolution limit [Å]	2.237	2.237
Rmerge	0.093	0.656
Number of reflections	39108
<I/σ(I)>	9.76	1.78
Completeness [%]	98.0	90
Redundancy	3.3	2.9
CC(1/2)	0.996	0.685

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		277	PROTEIN STOCK SOLUTION: 5.5 MG/ML CK2ALPHA'-D39G-C336S 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: 25 % PEG4000, 15 % glycerol, 0.17 M sodium acetate, 0.08 M Tris/HCl, pH 8.5; DROP SOLUTION BEFORE EQULIBRATION: 0.3 MICROLITER PROTEIN/INHIBITOR COMPLEX SOLUTION + 0.3 MICROLITER RESERVOIR SOLUTION