4D13

Crystal structure of cofactor-free urate oxidase in complex with its 5-peroxoisourate intermediate (X-ray dose, 2.2 kGy)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I02
Synchrotron site	Diamond
Beamline	I02
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-12-08
Detector	DECTRIS PILATUS 6M
Spacegroup name	I 2 2 2
Unit cell lengths	79.930, 95.080, 104.060
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	39.970 - 1.300
R-factor	0.10883
Rwork	0.108
R-free	0.13155
Structure solution method	OTHER
Starting model (for MR)	NONE
RMSD bond length	0.009
RMSD bond angle	1.447
Data reduction software	XDS
Data scaling software	Aimless
Refinement software	REFMAC (5.8.0069)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	1.330
High resolution limit [Å]	1.300	1.300
Rmerge	0.100	0.620
Number of reflections	96758
<I/σ(I)>	9.8	2.4
Completeness [%]	99.6	98.6
Redundancy	6.6	6.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1		8		20MG/ML UOX IN 50 MM TRIS-ACETATE PH 8.0 SATURATED WITH 9-METHYL URIC ACID UNDER ANAEROBIC CONDITIONS RESERVOIR: 8% PEG 8000, 50 MM TRIS-ACETATE PH 8.0 CRYSTALLIZATION WAS CARRIED OUT ANAEROBICALLY. CRYSTALS WERE INCUBATED WITH A RESERVOIR SOLUTION ENRICHED BY 10 MM H2O2 AND 20% GLYCEROL TO GENERATE THE PEROXIDE