6PX9

Crystal structure of procaspase-8 in complex with covalent small molecule inhibitor 63-R

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL9-2
Synchrotron site	SSRL
Beamline	BL9-2
Temperature [K]	100
Detector technology	PIXEL
Collection date	2016-02-12
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.98
Spacegroup name	P 31
Unit cell lengths	101.311, 101.311, 175.547
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	35.100 - 2.880
R-factor	0.2894
Rwork	0.286
R-free	0.36650
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4jj7
RMSD bond length	0.003
RMSD bond angle	0.677
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER
Refinement software	PHENIX (1.12_2829)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.930
High resolution limit [Å]	2.877	2.880
Rmerge	0.297	1.320
Rmeas	0.336	1.500
Rpim	0.156	0.710
Number of reflections	45476	2243
<I/σ(I)>	8.1	1.7
Completeness [%]	99.5	99.5
Redundancy	4.5	4.4
CC(1/2)	0.679	0.174

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8	293	0.1 M imidazole, pH 8.0, 1.0 M sodium citrate