5ZJ6

Crystal structure of HCK kinase complexed with a pyrrolo-pyrimidine inhibitor 7-[trans-4-(4-methylpiperazin-1-yl)cyclohexyl]-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SPRING-8 BEAMLINE BL26B2
Synchrotron site	SPring-8
Beamline	BL26B2
Temperature [K]	100
Detector technology	CCD
Collection date	2014-10-06
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1
Spacegroup name	P 1
Unit cell lengths	42.810, 48.020, 78.010
Unit cell angles	87.59, 83.09, 63.59

Refinement procedure

Resolution	38.094 - 1.696
R-factor	0.2078
Rwork	0.207
R-free	0.24010
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2hk5
RMSD bond length	0.004
RMSD bond angle	0.656
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER (2.8.0)
Refinement software	PHENIX (1.12_2829)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	38.094	38.094	1.800
High resolution limit [Å]	1.696	5.060	1.700
Rmerge	0.060	0.032	0.452
Rmeas	0.085	0.045	0.638
Total number of observations	112062
Number of reflections	56349	2210	8895
<I/σ(I)>	8.4	19.14	1.67
Completeness [%]	92.1	95.5	90
Redundancy	1.989	1.99	1.954
CC(1/2)	0.995	0.996	0.725

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		288	0.1 M Tris-HCl (pH 8.5) 25 % (v/v) PEG 10,000