6XE4

BTK Fluorocyclopropyl amide inhibitor, Compound 25

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 21-ID-F
Synchrotron site	APS
Beamline	21-ID-F
Temperature [K]	93
Detector technology	CCD
Collection date	2014-04-09
Detector	RAYONIX MX225-HS
Wavelength(s)	0.97872
Spacegroup name	P 61
Unit cell lengths	108.280, 108.280, 42.202
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	33.284 - 1.600
R-factor	0.1589
Rwork	0.158
R-free	0.18040
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	Null
RMSD bond length	0.005
RMSD bond angle	0.792
Data reduction software	HKL-2000
Data scaling software	SCALEPACK
Phasing software	PHASER
Refinement software	PHENIX (1.16-3549-000)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	35.000	35.000	1.630
High resolution limit [Å]	1.600	4.340	1.600
Rmerge	0.085	0.041	0.802
Rmeas	0.091	0.043	0.876
Rpim	0.032	0.016	0.346
Total number of observations	281402
Number of reflections	37127	1965	1758
<I/σ(I)>	7.7
Completeness [%]	98.8	99.8	93.9
Redundancy	7.6	7.8	6
CC(1/2)		0.998	0.541

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	7	291	PEG 10000, Li2SO4, pH 7.0