3VS6

Crystal structure of HCK complexed with a pyrazolo-pyrimidine inhibitor tert-butyl {4-[4-amino-1-(propan-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-3-yl]-2-methoxyphenyl}carbamate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SPRING-8 BEAMLINE BL32XU
Synchrotron site	SPring-8
Beamline	BL32XU
Temperature [K]	100
Detector technology	CCD
Collection date	2011-12-09
Detector	RAYONIX MX225HE
Wavelength(s)	1
Spacegroup name	P 21 21 21
Unit cell lengths	74.613, 96.392, 182.125
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	47.090 - 2.373
R-factor	0.2326
Rwork	0.230
R-free	0.28010
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3vry
RMSD bond length	0.007
RMSD bond angle	0.974
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER
Refinement software	PHENIX ((phenix.refine: 1.7.3_928))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.450
High resolution limit [Å]	2.370	2.370
Number of reflections	51828
<I/σ(I)>		2.1
Completeness [%]	99.9	99.6
Redundancy		9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	9	277	0.1M Tris, 0.1M calcium acetate, 20% glycerol, 21% PEG6000, pH 9, VAPOR DIFFUSION, SITTING DROP, temperature 277K