8FF0

Structure of BTK kinase domain with the second-generation inhibitor tirabrutinib

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 24-ID-E
Synchrotron site	APS
Beamline	24-ID-E
Temperature [K]	100
Detector technology	PIXEL
Collection date	2022-07-07
Detector	DECTRIS EIGER2 X 16M
Wavelength(s)	0.97918
Spacegroup name	P 61
Unit cell lengths	108.187, 108.187, 45.172
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	19.410 - 2.600
R-factor	0.2423
Rwork	0.241
R-free	0.26670
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.003
RMSD bond angle	0.805
Data reduction software	autoPROC
Data scaling software	autoPROC
Phasing software	PHASER
Refinement software	PHENIX (1.20.1_4487)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	19.410	2.705
High resolution limit [Å]	2.600	2.603
Rmerge	0.064
Rmeas	0.068
Rpim	0.022	0.685
Number of reflections	8801	440
<I/σ(I)>	17.2	1.1
Completeness [%]	93.5	44
Redundancy	9.9	9.9
CC(1/2)	0.999	0.455

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.5	277	16% PEG 8000 and 0.1M sodium citrate