4UXL

Structure of Human ROS1 Kinase Domain in Complex with PF-06463922

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	87
Detector technology	PIXEL
Collection date	2012-04-19
Detector	DECTRIS PILATUS 6M
Spacegroup name	P 64
Unit cell lengths	105.844, 105.844, 49.843
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	91.660 - 2.400
R-factor	0.211
Rwork	0.211
R-free	0.28100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3zbf
RMSD bond length	0.006
RMSD bond angle	0.900
Data reduction software	autoPROC
Data scaling software	SCALA
Phasing software	CNX
Refinement software	CNS (2005)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	91.660	2.330
High resolution limit [Å]	2.210	2.210
Rmerge	0.040	0.420
Number of reflections	15684
<I/σ(I)>	27	2.8
Completeness [%]	97.1	62.1
Redundancy	6.7	4.4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.6	286	CRYSTALS WERE OBTAINED BY THE HANGING DROP VAPOR DIFFUSION METHOD AT 13 DEGREES C BY MIXING 1.5 MICROLITERS OF SOLUTION CONTAINING A 1:3 MOLAR RATIO OF PHOSPHORYLATED ROS1 KD (12.2MG/ML) TO PF-06463922 AND 1.5 MICROLITERS OF RESERVOIR SOLUTION CONTAINING 25% (W/V) PEG 3350, 0.6M POTASSIUM THIOCYANATE AND 0.1M SODIUM CITRATE TRIBASIC DIHYDRATE, PH5.6. CRYSTALS WERE FLASH-FROZEN IN LIQUID NITROGEN AFTER TRANSFER TO 2 MICROLITERS OF RESERVOIR SOLUTION CONTAINING 25% (V/V) GLYCEROL AS A CRYOPROTECTANT.