6YG2

Crystal structure of MKK7 (MAP2K7) in complex with ibrutnib, with covalent and allosteric binding modes

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I04
Synchrotron site	Diamond
Beamline	I04
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-10-13
Detector	DECTRIS PILATUS3 6M
Wavelength(s)	1.02823
Spacegroup name	P 21 21 21
Unit cell lengths	53.111, 74.955, 86.666
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	19.550 - 2.000
R-factor	0.1815
Rwork	0.179
R-free	0.23040
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2dyl
RMSD bond length	0.015
RMSD bond angle	1.491
Data reduction software	XDS
Data scaling software	SCALA (3.3.21)
Phasing software	PHASER
Refinement software	REFMAC (5.8.0073)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	19.550	19.380	2.110
High resolution limit [Å]	2.000	6.320	2.000
Rmerge	0.106	0.045	0.901
Rmeas	0.115	0.050	0.968
Rpim	0.042	0.020	0.351
Number of reflections	24057	825	3473
<I/σ(I)>	12.1	11	0.8
Completeness [%]	99.9	96.6	100
Redundancy	7.3	6.5	7.4
CC(1/2)	0.997		0.901

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.8	277.15	19% PEG3350, 0.1 M ammonium acetate, 0.1 M tris, pH 7.8