4KSP

Crystal Structure of Human B-raf bound to a DFG-out Inhibitor TAK-632

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 23-ID-B
Synchrotron site	APS
Beamline	23-ID-B
Temperature [K]	92
Detector technology	CCD
Collection date	2010-06-13
Detector	MARMOSAIC 300 mm CCD
Wavelength(s)	1
Spacegroup name	P 41 21 2
Unit cell lengths	111.495, 111.495, 145.487
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	35.000 - 2.930
R-factor	0.1965
Rwork	0.194
R-free	0.24170
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4dbn
RMSD bond length	0.007
RMSD bond angle	1.317
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	MOLREP
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	3.000
High resolution limit [Å]	2.930	8.000	2.930
Rmerge	0.157	0.058	0.861
Number of reflections	20267
<I/σ(I)>	5.4
Completeness [%]	99.8	99.4	98.5
Redundancy	6.7	6.3	3.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	sitting drop, vapor diffusion	8.3	277	9.6 % PEG 8000, 0.8M LiCl, 100 mM Tris pH 8.3, sitting drop, vapor diffusion, temperature 277K