5M56
Monoclinic complex structure of human protein kinase CK2 catalytic subunit (isoform CK2alpha') with the inhibitor 4'-carboxy-6,8-chloro-flavonol (FLC21)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | SLS BEAMLINE X06DA |
Synchrotron site | SLS |
Beamline | X06DA |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2012-10-20 |
Detector | DECTRIS PILATUS3 2M |
Wavelength(s) | 1.00000 |
Spacegroup name | P 1 21 1 |
Unit cell lengths | 69.341, 87.620, 72.977 |
Unit cell angles | 90.00, 109.69, 90.00 |
Refinement procedure
Resolution | 43.810 - 2.237 |
R-factor | 0.1648 |
Rwork | 0.164 |
R-free | 0.20630 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 3ofm |
RMSD bond length | 0.002 |
RMSD bond angle | 0.516 |
Data reduction software | XDS |
Data scaling software | Aimless |
Phasing software | PHENIX |
Refinement software | PHENIX ((1.10.1_2155: ???)) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 44.000 | 2.317 |
High resolution limit [Å] | 2.237 | 2.237 |
Rmerge | 0.093 | 0.656 |
Number of reflections | 39108 | |
<I/σ(I)> | 9.76 | 1.78 |
Completeness [%] | 98.0 | 90 |
Redundancy | 3.3 | 2.9 |
CC(1/2) | 0.996 | 0.685 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 277 | PROTEIN STOCK SOLUTION: 5.5 MG/ML CK2ALPHA'-D39G-C336S IN 0.5 M NACL, 25 MM TRIS/HCL, PH 8.5; INHIBITOR STOCK SOLUTION: 10 MM INHIBITOR IN DMSO; PROTEIN/INHIBITOR COMPLEX SOLUTION: 90 MICROLITER PROTEIN STOCK SOLUTION + 10 MICROLITER INHIBITOR STOCK SOLUTION; RESERVOIR SOLUTION: 25 % PEG4000, 15 % glycerol, 0.17 M sodium acetate, 0.08 M Tris/HCl, pH 8.5; DROP SOLUTION BEFORE EQULIBRATION: 0.3 MICROLITER PROTEIN/INHIBITOR COMPLEX SOLUTION + 0.3 MICROLITER RESERVOIR SOLUTION |