5EH0

Rapid Discovery of Pyrido[3,4-d]pyrimidine Inhibitors of Monopolar Spindle kinase 1 (MPS1) Using a Structure-Based Hydridization Approach

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
Wavelength(s)	0.9680
Spacegroup name	I 2 2 2
Unit cell lengths	70.420, 105.920, 112.210
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	23.780 - 2.180
R-factor	0.1975
Rwork	0.196
R-free	0.21650
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	1.060
Data reduction software	XDS
Data scaling software	Aimless (0.5.7)
Phasing software	PHASER (2.5.7)
Refinement software	BUSTER-TNT

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	40.540	40.540	2.250
High resolution limit [Å]	2.180	8.990	2.180
Rmerge	0.042	0.020	2.555
Rpim	0.022	0.011	1.393
Total number of observations	97927	1396	8221
Number of reflections	22272
<I/σ(I)>	11.4	41.4	0.5
Completeness [%]	99.9	99.3	99.7
Redundancy	4.4	3.8	4.3
CC(1/2)	0.999	0.999	0.374

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	291.15	0.1 M BisTris Propane pH 7.5 0.2 M MgCl2 0.2M Sodium Formate 20% PEG3350