5H09

Crystal structure of HCK complexed with a pyrrolo-pyrimidine inhibitor (S)-ethyl2-(((1r,4S)-4-(4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)cyclohexyl)amino)-4-methylpentanoate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	PHOTON FACTORY BEAMLINE AR-NE3A
Synchrotron site	Photon Factory
Beamline	AR-NE3A
Temperature [K]	100
Detector technology	CCD
Collection date	2014-02-16
Detector	ADSC QUANTUM 270
Wavelength(s)	0.91
Spacegroup name	P 21 21 21
Unit cell lengths	43.037, 85.425, 128.840
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	28.640 - 1.945
R-factor	0.1917
Rwork	0.190
R-free	0.22270
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3vs3
RMSD bond length	0.003
RMSD bond angle	0.631
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER (2.5.5)
Refinement software	PHENIX (1.11.1_2575)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.980
High resolution limit [Å]	1.950	5.290	1.950
Rmerge	0.116	0.070	0.914
Rmeas	0.126	0.077	0.986
Rpim	0.047	0.031	0.367
Total number of observations	254528
Number of reflections	35580	1921	1747
<I/σ(I)>	7.4
Completeness [%]	99.9	97.6	100
Redundancy	7.2	6.1	7.2
CC(1/2)		0.995	0.777

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	0.22-0.25 M ammonium formate, 12-22 % PEG 3350