9SPZ

Crystal structure of the Molybdenum-containing nitrogenase from Methanocaldococcus infernus refined to 1.37 A resolution - crystalline form A

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X06SA
Synchrotron site	SLS
Beamline	X06SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2022-10-12
Detector	DECTRIS EIGER X 16M
Wavelength(s)	1.00000
Spacegroup name	P 1 21 1
Unit cell lengths	78.433, 117.180, 106.627
Unit cell angles	90.00, 91.48, 90.00

Refinement procedure

Resolution	21.910 - 1.370
R-factor	0.1249
Rwork	0.123
R-free	0.15560
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.011
RMSD bond angle	1.262
Data reduction software	autoPROC
Data scaling software	autoPROC
Phasing software	PHASER
Refinement software	PHENIX ((1.21.2_5419: ???))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	78.850	1.515
High resolution limit [Å]	1.370	1.370
Rmerge	0.091	1.198
Rmeas	0.096	1.266
Rpim	0.029	0.404
Number of reflections	273586	13675
<I/σ(I)>	12.3	1.9
Completeness [%]	95.3	68.2
Redundancy	10.4	9.6
CC(1/2)	0.998	0.658

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	8.5	293.15	Samples were centrifuged at 13,000 x g for 3 min to remove macro-aggregates and dust, and crystallised inside an anaerobic chamber (N2/H2 (97:3%) atmosphere, 20 degrees Celsius). Crystallisation was done by the sitting drop method in 96-Well MRC 2-Drop polystyrene Crystallisation Plates (SWISSCI) plate containing 90 uL of crystallisation solution in the reservoir in all cases. Crystals were obtained by mixing 0.7 uL of crystallisation solution with 0.7 uL of protein sample at a concentration of 2.95 mg/mL. The crystallisation solution contained the following: 30 % v/v 2-methyl-2,4-pentanediol, 100 mM Tris pH 8.5, 500 mM Sodium chloride, and 8 % w/v Polyethylene glycol 8,000 (Crystallisation solution of the JBScreen Wizard form Jena Bioscience, Germany).