3V5L

Crystal Structure of Interleukin-2 Inducible T-cell Kinase Itk Catalytic Domain with Thienopyrazolylindole Inhibitor 542

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID14-1
Synchrotron site	ESRF
Beamline	ID14-1
Temperature [K]	100
Detector technology	CCD
Collection date	2005-06-22
Detector	ADSC QUANTUM 4
Wavelength(s)	0.934
Spacegroup name	P 1 21 1
Unit cell lengths	68.974, 68.912, 140.025
Unit cell angles	90.00, 100.52, 90.00

Refinement procedure

Resolution	47.580 - 1.860
R-factor	0.2324
Rwork	0.232
R-free	0.25190
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1sm2
RMSD bond length	0.007
RMSD bond angle	0.960
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	PHASER
Refinement software	BUSTER-TNT (BUSTER 2.9.1)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.930
High resolution limit [Å]	1.860	4.010	1.860
Rmerge	0.059	0.028	0.511
Number of reflections	106608
<I/σ(I)>	9
Completeness [%]	98.5	99.1	94.3
Redundancy	3	3.4	2.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	6	294	0.8M Ammonium-sulfate, 0.1 M Na-citrate, 0.225 M Mg-acetate, 4% acetone, 10 mM DTT, pH 6.0, VAPOR DIFFUSION, temperature 294K