4FBX

Complex structure of human protein kinase CK2 catalytic subunit crystallized in the presence of a bisubstrate inhibitor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SEALED TUBE
Source details	OTHER
Temperature [K]	100
Detector technology	CCD
Collection date	2010-12-14
Detector	AGILENT ATLAS CCD
Wavelength(s)	1.5418
Spacegroup name	P 43 21 2
Unit cell lengths	72.114, 72.114, 135.056
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	31.807 - 2.330
R-factor	0.2018
Rwork	0.199
R-free	0.24920
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.003
RMSD bond angle	0.677
Data reduction software	XDS
Data scaling software	SCALA
Phasing software	PHENIX
Refinement software	PHENIX ((phenix.refine: 1.7.3_928))

Data quality characteristics

	Overall
Low resolution limit [Å]	32.250
High resolution limit [Å]	2.330
Rmerge	0.095
Number of reflections	15925
<I/σ(I)>	18.8
Completeness [%]	99.9
Redundancy	8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	The concentrated enzyme solution contained 6.2 mg/ml protein dissolved in 500 mM NaCl, 25 mM Tris/HCl, pH 8.5. Nine volume parts of this protein stock solution were mixed with one part 12 mM ARC-1154 dissolved in 100% dimethyl sulfoxide. The CK2alpha1-335/ARC-1154 mixture was incubated for 30 min at room temperature. The best crystals grew with a reservoir solution composed of 4.4 M NaCl, 100 mM citric acid, pH 5.25 and mixing 2 microliter of this reservoir solution with microliter CK2alpha1-335/ARC-1154 mixture, VAPOR DIFFUSION, SITTING DROP, temperature 293K