8U2D

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	2018-06-15
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0
Spacegroup name	P 21 21 21
Unit cell lengths	38.390, 79.340, 106.880
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	44.320 - 1.950
R-factor	0.1928
Rwork	0.191
R-free	0.23840
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.007
RMSD bond angle	0.873
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]	44.320	2.020
High resolution limit [Å]	1.950	1.950
Rmerge	0.228	1.922
Rmeas	0.247	2.079
Rpim	0.096	0.786
Number of reflections	24245	2338
<I/σ(I)>	7.76	1.1
Completeness [%]	98.6	96.93
Redundancy	6.6	6.9
CC(1/2)	0.992	0.374

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	277	30% EDO_P8K, 0.03M NaF, 0.03M, NaBr, 0.03M NaI, 0.05M Sodium HEPES, 0.05M MOPS pH 7.5