7A22
Crystal structure of human protein kinase CK2alpha' (CSNK2A2 gene product) in complex with the ATP-competitive inhibitor 5,6,7-tribromo-1H-triazolo[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 | 46.501, 47.696, 50.571 |
Unit cell angles | 113.15, 90.46, 90.27 |
Refinement procedure
Resolution | 46.500 - 1.010 |
R-factor | 0.1382 |
Rwork | 0.138 |
R-free | 0.16600 |
Structure solution method | AB INITIO PHASING |
RMSD bond length | 0.012 |
RMSD bond angle | 1.353 |
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] | 46.500 | 1.106 |
High resolution limit [Å] | 1.008 | 1.008 |
Rmerge | 0.071 | 0.991 |
Rmeas | 0.077 | 1.114 |
Rpim | 0.030 | 0.495 |
Number of reflections | 149108 | 7455 |
<I/σ(I)> | 11.7 | 1.5 |
Completeness [%] | 70.8 | |
Redundancy | 6.4 | |
CC(1/2) | 0.998 | 0.555 |
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-triazolo[4,5-b]pyridine by extensive crystal soaking. |