7N5O

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	2012-02-29
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.976
Spacegroup name	P 21 21 2
Unit cell lengths	72.662, 104.599, 38.034
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.000 - 1.250
R-factor	0.1794
Rwork	0.179
R-free	0.19590
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4z3v
RMSD bond length	0.007
RMSD bond angle	1.567
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	1.270
High resolution limit [Å]	1.250	3.390	1.250
Rmerge	0.079	0.049	0.689
Total number of observations	520829
Number of reflections	74258	4338	2038
<I/σ(I)>	9.2
Completeness [%]	91.6	99.3	51
Redundancy	7	6.9	4.9

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