4LUE

Crystal Structure of HCK in complex with 7-[trans-4-(4-methylpiperazin-1-yl)cyclohexyl]-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine (resulting from displacement of SKF86002)

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	2013-02-01
Detector	RAYONIX MX-225
Wavelength(s)	1.0
Spacegroup name	P 21 21 21
Unit cell lengths	73.400, 93.530, 181.490
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	46.765 - 3.040
R-factor	0.208
Rwork	0.205
R-free	0.25620
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3vs3
RMSD bond length	0.003
RMSD bond angle	0.646
Data reduction software	MOSFLM
Data scaling software	SCALA (3.3.20)
Phasing software	PHASER (2.5.2)
Refinement software	PHENIX (1.8.2_1309)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	90.745	57.068	3.200
High resolution limit [Å]	3.040	9.610	3.040
Rmerge		0.034	0.374
Rmeas		0.037	0.405
Rpim		0.014	0.153
Total number of observations		5729	24488
Number of reflections	24812
<I/σ(I)>	12.5	22.3	5
Completeness [%]	100.0	99.5	100
Redundancy	7	6.4	6.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8	288	0.1M Tris, 0.1M Calcium Acetate, 20% Glycerol, 24% PEG 6000, 2mM SKF86002, soaked with 2mM inhibitor in DMSO., pH 8.0, VAPOR DIFFUSION, SITTING DROP, temperature 288K