5M4U

ORTHORHOMBIC 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 PILATUS 2M
Wavelength(s)	1.0000
Spacegroup name	P 21 21 21
Unit cell lengths	46.850, 83.780, 142.344
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	44.502 - 2.195
R-factor	0.1721
Rwork	0.170
R-free	0.21400
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3ofm
RMSD bond length	0.003
RMSD bond angle	0.576
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]	44.600	2.274
High resolution limit [Å]	2.195	2.195
Rmerge	0.191	1.185
Number of reflections	29246
<I/σ(I)>	9.99	1.72
Completeness [%]	99.0	93
Redundancy	6.4	5.6
CC(1/2)	0.998	0.684

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	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 % PEG5000 MME, 0.2 M ammonium sulphate, 0.1 M MES buffer, pH 6.5; DROP SOLUTION BEFORE EQULIBRATION: 0.3 MICROLITER PROTEIN/INHIBITOR COMPLEX SOLUTION + 0.3 MICROLITER RESERVOIR SOLUTION