6YZ4

Crystal structure of MKK7 (MAP2K7) with ibrutinib bound at allosteric site

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	2014-10-04
Detector	DECTRIS PILATUS3 6M
Wavelength(s)	1.02823
Spacegroup name	P 21 21 21
Unit cell lengths	53.510, 74.670, 87.170
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	25.535 - 1.700
R-factor	0.1711
Rwork	0.169
R-free	0.20610
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2dyl
RMSD bond length	0.016
RMSD bond angle	1.610
Data reduction software	iMOSFLM
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]	25.535	25.535	1.790
High resolution limit [Å]	1.700	5.380	1.700
Rmerge	0.085	0.029	0.781
Rmeas	0.092	0.031	0.849
Rpim	0.036	0.012	0.328
Number of reflections	39163	1359	5630
<I/σ(I)>	13.1	20.7	2.3
Completeness [%]	99.9	99	99.9
Redundancy	6.5	6	6.5
CC(1/2)	0.999		0.552

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.8	277.15	16% PEG3350, 0.1 M tris pH 7.8, 0.25 M ammonium acetate