7N5R

Fragment-Based Discovery of a Novel Bruton's Tyrosine Kinase Inhibitor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.3
Synchrotron site	ALS
Beamline	5.0.3
Temperature [K]	100
Detector technology	CCD
Collection date	2011-05-13
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.976
Spacegroup name	P 21 21 2
Unit cell lengths	72.692, 104.682, 38.058
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.000 - 1.550
R-factor	0.1725
Rwork	0.171
R-free	0.19500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4z3v
RMSD bond length	0.008
RMSD bond angle	1.528
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	MOLREP
Refinement software	REFMAC (5.8.0267)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.530
High resolution limit [Å]	1.500	4.070	1.500
Rmerge	0.089	0.036	0.539
Total number of observations	297351
Number of reflections	46122	2574	1752
<I/σ(I)>	9.6
Completeness [%]	97.9	100	75.3
Redundancy	6.4	6.5	3.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5	277	10% polyethylene glycol 4000, 20% glycerol, 0.1M imidazole/MES, pH 6.5 and 0.12M alcohol mixture