7UP6

Crystal structure of C-terminal domain of MSK1 in complex with in covalently bound literature RSK2 inhibitor pyrrolopyrimidine cyanoacrylamide compound 25 (co-crystal)

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	2018-03-08
Detector	RAYONIX MX-300
Wavelength(s)	0.97872
Spacegroup name	P 61
Unit cell lengths	71.170, 71.170, 144.840
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	35.590 - 2.600
R-factor	0.17
Rwork	0.166
R-free	0.20900
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	in-house model
RMSD bond length	0.004
RMSD bond angle	0.593
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (1.13)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	35.590	2.670
High resolution limit [Å]	2.600	2.600
Rmerge	0.084	0.575
Rmeas	0.090	0.037
Total number of observations	98583
Number of reflections	12830	154
<I/σ(I)>	17.02	2.82
Completeness [%]	99.9	100
Redundancy	7.7	7.5
CC(1/2)	0.999	0.999

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	289	Crystals were produced by sitting drop vapor diffusion with an equal volume of the protein, Msk1-C terminal domain (PID6598-1, CID101276) at 4.91 mg/ml in 25mM HEPES pH 7.5, 150mM NaCl, 5% Glycerol, 5mM BME and a crystallization buffer containing 12.5% PEG 1000, 12.5% PEG 3350, 12.5% MPD: 20mM of each sodium formate, ammonium acetate, trisodium citrate, sodium-potassium tartrate, sodium oxamate: 100 mM MOPS / HEPES-Na pH 7.5 (tray ID 298849, well G8, Morpheus). Crystals were direly vitrified in in liquid N2. Puck ID BOW0-8