2V3V

A New Catalytic Mechanism of Periplasmic Nitrate Reductase from Desulfovibrio desulfuricans ATCC 27774 from Crystallographic and EPR Data and based on detailed analysis of the sixth ligand

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE ID14-3
Synchrotron site	ESRF
Beamline	ID14-3
Temperature [K]	100
Detector technology	CCD
Collection date	2004-11-22
Detector	ADSC CCD
Spacegroup name	P 31 2 1
Unit cell lengths	106.566, 106.566, 135.479
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	92.450 - 1.990
R-factor	0.185
Rwork	0.182
R-free	0.24600
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2nap
RMSD bond length	0.013
RMSD bond angle	1.698
Data reduction software	MOSFLM
Data scaling software	SCALEPACK
Refinement software	REFMAC (5.2.0019)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	46.130	2.010
High resolution limit [Å]	1.910	1.910
Rmerge	0.114	1.330
Number of reflections	454081
<I/σ(I)>	10	0.8
Completeness [%]	93.5	60.4
Redundancy	7	2.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1		6.5		0.1M MES, PH 6.5, 7.5% PEG 8000 A COCRYSTALLISATION WITH 10MM OF KCLO4 (PERCHLORATE) IN 200MM OF DDNAPA (IE PROTEIN) WHICH HAD BEEN REDUCED BY DITHIONITE IN ANAEROBIC CONDITIONS AND THEN AIR REOXIDISED BEFORE SETTTING UP FOR CRYSTALLISATIONS STRAIGHT AFTER THAWING FROM -80C.