7A2H
Crystal structure of human protein kinase CK2alpha' (CSNK2A2 gene product) in complex with the ATP-competitive inhibitor 5,6,7-tribromo-1H-imidazo[4,5-b]pyridine
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 | 2018-11-14 |
Detector | DECTRIS PILATUS 2M |
Wavelength(s) | 0.87313 |
Spacegroup name | P 1 |
Unit cell lengths | 46.826, 47.604, 50.486 |
Unit cell angles | 67.15, 89.52, 89.29 |
Refinement procedure
Resolution | 46.820 - 1.010 |
R-factor | 0.1427 |
Rwork | 0.143 |
R-free | 0.14950 |
Structure solution method | AB INITIO PHASING |
RMSD bond length | 0.008 |
RMSD bond angle | 1.043 |
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] | 46.822 | 1.090 |
High resolution limit [Å] | 1.010 | 1.010 |
Rmerge | 0.064 | 0.909 |
Rmeas | 0.068 | 0.999 |
Rpim | 0.022 | 0.399 |
Number of reflections | 159561 | 7978 |
<I/σ(I)> | 16.2 | 1.5 |
Completeness [%] | 75.8 | 18.5 |
Redundancy | 9.1 | 5.7 |
CC(1/2) | 0.999 | 0.650 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 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 initial inhibitor MB002 was replaced by the inhibitor 5,6,7-tribromo-1H-imidazo[4,5-b]pyridine by extensive crystal soaking. |