4WHQ

Alkylperoxo reaction intermediate trapped in Protocatechuate 3,4-dioxygenase (pseudomonas putida) at pH 6.5

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 19-ID
Synchrotron site	APS
Beamline	19-ID
Temperature [K]	100
Detector technology	CCD
Collection date	2014-07-11
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.97918
Spacegroup name	I 2 2 2
Unit cell lengths	128.259, 140.724, 167.824
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	39.010 - 1.780
R-factor	0.1658
Rwork	0.164
R-free	0.19510
RMSD bond length	0.011
RMSD bond angle	1.522
Data reduction software	HKL-3000
Data scaling software	HKL-3000
Refinement software	REFMAC (5.7.0029)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.810
High resolution limit [Å]	1.780	4.830	1.780
Rmerge	0.073	0.037	0.479
Rmeas	0.082	0.041	0.547
Rpim	0.036	0.018	0.255
Total number of observations	671887
Number of reflections	140459
<I/σ(I)>	16.4
Completeness [%]	97.7	86.9	97.2
Redundancy	4.8	5	4.1
CC(1/2)		0.997	0.811

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5	295	1.2 M Ammonium Sulfate, 2.5 mM 2-mercaptoethanol, 100 mM MES pH 6.5; 2:1 ratio of well sol. to 40 mg/ml protein solution in drop