6HMB
STRUCTURE OF PROTEIN KINASE CK2 CATALYTIC SUBUNIT (ISOFORM CK2ALPHA'; CSNK2A2 Gene product) IN COMPLEX WITH the inhibitor CX-4945 (Silmitasertib)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | ESRF BEAMLINE ID30B |
Synchrotron site | ESRF |
Beamline | ID30B |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2018-07-16 |
Detector | DECTRIS PILATUS3 S 6M |
Wavelength(s) | 0.8 |
Spacegroup name | P 1 |
Unit cell lengths | 46.350, 47.720, 50.420 |
Unit cell angles | 113.08, 90.28, 90.85 |
Refinement procedure
Resolution | 32.592 - 1.040 |
R-factor | 0.1345 |
Rwork | 0.134 |
R-free | 0.14630 |
Structure solution method | AB INITIO PHASING |
RMSD bond length | 0.009 |
RMSD bond angle | 1.180 |
Data reduction software | XDS |
Data scaling software | XSCALE |
Phasing software | Arcimboldo |
Refinement software | PHENIX ((1.13_2998: ???)) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 32.750 | 1.077 |
High resolution limit [Å] | 1.040 | 1.040 |
Rmerge | 0.071 | 1.286 |
Rmeas | 0.077 | 1.398 |
Rpim | 0.030 | 0.541 |
Number of reflections | 187923 | 18488 |
<I/σ(I)> | 11.75 | 1.5 |
Completeness [%] | 98.3 | 96.75 |
Redundancy | 6.5 | 6.4 |
CC(1/2) | 0.998 | 0.576 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 8.5 | 293.15 | 180 MICROLITER ENZYME STOCK SOLUTION (6 MG/ML IN 500 MM NACL, 25 MM TRIS/HCL, PH 8.5) WERE MIXED and incubated WITH 20 MIKROLITER of a STOCK SOLUTION of the inhibitor 4B0 (10 MM 4B0 IN DMSO). 20 MICROLITERS OF the resulting solution WERE MIXED WITH 10 MICROLITERS OF RESERVOIR SOLUTION (900 MM LICL, 28 % (W/V) PEG 6000, 100 MM TRIS/HCL, PH 8.5) IN EACH WELL OF A CRYSTALLIZATION PLATE. A SINGLE MACROSEED, grown UNDER THE SAME CONDITIONS, WAS ADDED TO EACH DROPLET of the plate. THE DROPLETS WERE EQUILIBRATED AT 293.15 K using the sitting drop variant of the VAPOR DIFFUSION method. This procedure generated large single crystals of a CK2alpha'/4B0 complex. Afterwards, the inhibitor 4B0 was exchanged against CX-4945 by an extensive soaking procedure of several steps. |