4PPB

ITK kinase domain with compound 28 (N-{1-[(1S)-3-(DIMETHYLAMINO)-1-PHENYLPROPYL]-1H-PYRAZOL-4-YL}-6-(1H-PYRAZOL-4-YL)-1H-INDAZOLE-3-CARBOXAMIDE)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL12-2
Synchrotron site	SSRL
Beamline	BL12-2
Temperature [K]	110
Detector technology	PIXEL
Collection date	2011-03-23
Detector	PSI PILATUS 6M
Wavelength(s)	0.9795
Spacegroup name	P 21 21 21
Unit cell lengths	39.937, 94.407, 156.206
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	40.400 - 2.820
R-factor	0.2138
Rwork	0.211
R-free	0.26610
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1sm2
RMSD bond length	0.008
RMSD bond angle	1.020
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	BUSTER (2.11.4)

Data quality characteristics

	Overall
Low resolution limit [Å]	40.400
High resolution limit [Å]	2.810
Number of reflections	14680
<I/σ(I)>	18.8
Completeness [%]	97.8
Redundancy	6.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8.5	280	sodium nitrate, PEG3350, pH 8.5, VAPOR DIFFUSION, HANGING DROP, temperature 380K