7AT9

Structure of protein kinase ck2 catalytic subunit (csnk2a2 gene product) in complex with the ATP-competitive inhibitor MB002 and the alphaD-pocket ligand 3,4-dichlorophenethylamine

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID23-2
Synchrotron site	ESRF
Beamline	ID23-2
Temperature [K]	100
Detector technology	PIXEL
Collection date	2018-11-15
Detector	DECTRIS PILATUS3 X 2M
Wavelength(s)	0.873127
Spacegroup name	P 1
Unit cell lengths	46.482, 47.661, 50.733
Unit cell angles	66.61, 89.44, 88.66

Refinement procedure

Resolution	43.740 - 1.050
R-factor	0.1293
Rwork	0.129
R-free	0.14960
Structure solution method	AB INITIO PHASING
RMSD bond length	0.010
RMSD bond angle	1.163
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	Arcimboldo
Refinement software	PHENIX (1.18.2_3874)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	46.565	1.103
High resolution limit [Å]	1.039	1.039
Rmerge	0.075	1.096
Rmeas	0.079	1.239
Rpim	0.025	0.558
Number of reflections	154027	7703
<I/σ(I)>	13.4	1.2
Completeness [%]	80.1	24.5
Redundancy	8.6	4.4
CC(1/2)	0.999	0.513

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8.5	293	Reservoir composition: 28 % (w/v) PEG6000, 0.9 M LiCl, 0.1 M, Tris/HCl, pH 8.5; drop composition prior to equilibration: 0.01 ml reservoir solution + 0.02 ml CK2alpha' (mutant Cys336Ser)/inhibitor MB002 mixture (0.180 ml 6 mg/ml CK2alpha'Cys336Ser, 0.5 M NaCl, 25 mM Tris/HCl, pH 8.5, mixed and pre-equilibrated with 0.02 ml 10 mM MB002 in dimethyl sulfoxide); the alphaD-pocket ligand 3,4-dichlorophenethylamine was introduced by extensive soaking.