4CTC

Structure of the Human Anaplastic Lymphoma Kinase in Complex with the inhibitor 7-amino-3-cyclopropyl-12-fluoro-1,10,16-trimethyl-16,17- dihydro-1H-8,4-(metheno)pyrazolo(4,3-h)(2,5,11) benzoxadiazacyclotetradecin-15(10H)-one

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I03
Synchrotron site	Diamond
Beamline	I03
Temperature [K]	87
Detector technology	PIXEL
Collection date	2012-02-03
Detector	DECTRIS PILATUS 6M
Spacegroup name	P 21 21 21
Unit cell lengths	51.810, 57.100, 104.710
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	52.350 - 2.030
R-factor	0.1938
Rwork	0.193
R-free	0.21570
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2xp2
RMSD bond length	0.009
RMSD bond angle	1.030
Data reduction software	CCP4
Data scaling software	SCALA
Phasing software	CNX
Refinement software	BUSTER (2.11.4)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	52.350	2.080
High resolution limit [Å]	2.030	2.030
Rmerge	0.120	0.580
Number of reflections	20763
<I/σ(I)>	10.2	2.7
Completeness [%]	99.9	99.6
Redundancy	6.5	6.4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.6	286	HANGING DROP VAPOR DIFFUSION AT 13 DEGREES C. EQUAL VOLUMES OF PURIFIED PROTEIN SOLUTION (APPROXIMATELY 13-15 MG/ML)CONTAINING 0.001M INHIBITOR COMPOUND WERE COMBINED WITH A SOLUTION CONTAINING: 0.15M AMMONIUM SULFATE, 9-10.5% MONOMETHYLETHER PEG5K AND 0.1M MES IN THE PH RANGE 5.3-6.5