7N5Y

Fragment-Based Drug Design of a Novel, Covalent 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	2012-12-01
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.976
Spacegroup name	P 21 21 2
Unit cell lengths	72.717, 104.729, 38.050
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	30.000 - 1.850
R-factor	0.1646
Rwork	0.163
R-free	0.20150
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4z3v
RMSD bond length	0.007
RMSD bond angle	1.426
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	1.850
High resolution limit [Å]	1.820	4.940	1.820
Rmerge	0.123	0.045	0.650
Total number of observations	151880
Number of reflections	26776	1483	1275
<I/σ(I)>	7.4
Completeness [%]	99.9	99.2	99
Redundancy	5.7	5.5	3.6

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