4CV8

MPS1 kinase with 3-aminopyridin-2-one inhibitors

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I24
Synchrotron site	Diamond
Beamline	I24
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-07-29
Detector	DECTRIS PILATUS 6M
Spacegroup name	I 2 2 2
Unit cell lengths	70.800, 110.300, 114.200
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	41.230 - 3.000
R-factor	0.1824
Rwork	0.180
R-free	0.22560
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2zmc
RMSD bond length	0.010
RMSD bond angle	1.150
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	BUSTER (2.11.4)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	41.230	3.180
High resolution limit [Å]	3.000	3.000
Rmerge	0.140
Number of reflections	9187
<I/σ(I)>	9.2	1
Completeness [%]	99.5	99.7
Redundancy	4.4	4.4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1		7.5	291	0.2M NACO2H, 0.1M BTP PH 7.5, 15% W/V PEG3350, 1% DMSO AND 1MM (N-(2-OXO-5-(PYRIDIN-4-YL)-1, 2-DIHYDROPYRIDIN-3-YL)-4-PIPERIDIN-1-YL)BENZAMIDE. THEN BACK-SOAK IN A NEW SOLUTION OF 0.19M NACO2H, 0.095M BTP PH 7.5, 14.25% PEG3350 AND 2MM 3-AMINO-5-(1-METHYL-1H-PYRAZOL-4-YL) PYRIDIN-2(1H)-ONE FOR 24H ALL AT 18 DEGREES C.