4CMU

Structure of the Human Anaplastic Lymphoma Kinase in Complex with the inhibitor (10R)-7-amino-12-fluoro-1,3,10,16-tetramethyl-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 I04-1
Synchrotron site	Diamond
Beamline	I04-1
Temperature [K]	87
Detector technology	PIXEL
Collection date	2011-09-25
Detector	DECTRIS PILATUS 6M
Spacegroup name	P 21 21 21
Unit cell lengths	51.830, 57.300, 104.940
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	52.470 - 1.800
R-factor	0.206
Rwork	0.206
R-free	0.22700
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2xp2
RMSD bond length	0.005
RMSD bond angle	0.800
Data reduction software	XDS
Data scaling software	SCALA
Phasing software	CNX
Refinement software	CNX (2005)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	57.300	1.720
High resolution limit [Å]	1.680	1.680
Rmerge	0.570	0.850
Number of reflections	68428
<I/σ(I)>	18.4	2.6
Completeness [%]	99.9	99.9
Redundancy	6.6	6.8

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.5	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.