8U2E

Bruton's tyrosine kinase in complex with N-[(2R)-1-[(3R)-3-(methylcarbamoyl)-1H,2H,3H,4H,9H-pyrido[3,4-b]indol-2-yl]-3-(3-methylphenyl)-1-oxopropan-2-yl]-1H-indazole-5-carboxamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.2
Synchrotron site	ALS
Beamline	5.0.2
Temperature [K]	100
Detector technology	PIXEL
Collection date	2018-08-17
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0
Spacegroup name	P 21 21 21
Unit cell lengths	38.150, 77.960, 106.000
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	43.830 - 1.900
R-factor	0.1931
Rwork	0.191
R-free	0.23770
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.008
RMSD bond angle	0.923
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX (1.20.1_4487)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	43.830	1.968
High resolution limit [Å]	1.900	1.900
Rmerge	0.284	2.106
Rmeas	0.304	2.246
Rpim	0.106	0.774
Number of reflections	25668	2472
<I/σ(I)>	7.57	0.97
Completeness [%]	99.9	99.52
Redundancy	8	8.2
CC(1/2)	0.991	0.338

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	277	30% EDO_P8K, 0.03M NaN03, 0.03M Na2HPO4 0.03M (NH4)2SO4, 0.05M Imidazole, 0.05M MES pH 6.5