5XFE

Luciferin-regenerating enzyme solved by SAD using XFEL (refined against 11,000 patterns)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	FREE ELECTRON LASER
Source details	SACLA BEAMLINE BL3
Synchrotron site	SACLA
Beamline	BL3
Temperature [K]	293
Detector technology	CCD
Collection date	2014-05-15
Detector	MPCCD
Wavelength(s)	0.984
Spacegroup name	P 21 21 21
Unit cell lengths	47.900, 77.030, 84.530
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	24.568 - 1.500
R-factor	0.1924
Rwork	0.192
R-free	0.21340
Structure solution method	SAD
RMSD bond length	0.007
RMSD bond angle	1.130
Data reduction software	CrystFEL
Data scaling software	CrystFEL
Phasing software	SHELXDE
Refinement software	PHENIX (1.9_1692)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	25.000	25.000	1.560
High resolution limit [Å]	1.500	3.118	1.500
Total number of observations	4354445
Number of reflections	93667
<I/σ(I)>	2.712658	4.87	0.48
Completeness [%]	96.7	100	71.46
Redundancy	46.4886	94.6	3.6
CC(1/2)	0.924	0.890	0.079

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	BATCH MODE	7.5	293	mixing purified LRE solution (27 mg/mL LRE, 10 mM HEPES pH 7.5, 0.1 M NaCl, 10% glycerol) and precipitant solution (35% PEG3350, 10% MPD, 0.1 M HEPES pH 7.5, 0.2 M MgCl2) at ratios between 1:2 and 1:1.6