7UP7
Crystal structure of C-terminal Domain of MSK1 in complex with covalently bound with literature RSK2 inhibitor indazole cyanoacrylamide compound 26 (soak)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | APS BEAMLINE 21-ID-F |
Synchrotron site | APS |
Beamline | 21-ID-F |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2018-12-13 |
Detector | RAYONIX MX-300 |
Wavelength(s) | 0.97872 |
Spacegroup name | P 21 21 21 |
Unit cell lengths | 50.930, 90.520, 135.580 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 47.680 - 2.800 |
R-factor | 0.1877 |
Rwork | 0.181 |
R-free | 0.24440 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | in-house model |
RMSD bond length | 0.003 |
RMSD bond angle | 0.591 |
Data reduction software | XDS |
Data scaling software | XSCALE |
Phasing software | PHENIX |
Refinement software | PHENIX (1.17.1_3660) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 2.870 |
High resolution limit [Å] | 2.800 | 12.520 | 2.800 |
Rmerge | 0.086 | 0.022 | 0.576 |
Rmeas | 0.095 | 0.026 | 0.637 |
Number of reflections | 16052 | 207 | 1170 |
<I/σ(I)> | 16.94 | 42.94 | 3 |
Completeness [%] | 99.8 | 94.5 | 100 |
Redundancy | 5.267 | 4.111 | 5.377 |
CC(1/2) | 0.998 | 0.999 | 0.853 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 8 | 289 | Crystals were produced by sitting drop vapor diffusion with an equal volume of the protein, Msk1-C terminal domain (PID7059-1, CID101276) at 5 mg/ml with 1.5mM UCB1590591/BSI106893 in 25mM HEPES pH 7.5, 150mM NaCl, 5% Glycerol, 5mM BME and a crystallization buffer containing 100mM sodium malonate pH 8.0, 100mM Tris pH 8.0, 30% w/v PEG 1000 (tray ID 305760, well F2, CID101276_fine1 screen). Crystals were soaked for 4 days in 2.5ul of reservoir with 1mM UCB1590956/BSI100006.Crystals were cryo protected with 20% EG + compound and vitrified in in liquid N2. Puck ID WJP9-1 |