9SQ3

Crystal structure of the Molybdenum-containing nitrogenase from Methanocaldococcus infernus refined to 1.21 A resolution - crystalline form B.

This is a non-PDB format compatible entry.

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE BM07
Synchrotron site	ESRF
Beamline	BM07
Temperature [K]	100
Detector technology	PIXEL
Collection date	2023-05-17
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.97951
Spacegroup name	P 1
Unit cell lengths	68.504, 80.243, 105.744
Unit cell angles	74.49, 82.25, 65.02

Refinement procedure

Resolution	33.620 - 1.210
R-factor	0.1221
Rwork	0.121
R-free	0.14600
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.013
RMSD bond angle	1.472
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]	101.860	1.350
High resolution limit [Å]	1.210	1.210
Rmerge	0.074	1.071
Rmeas	0.079	1.154
Rpim	0.030	0.425
Number of reflections	371908	18595
<I/σ(I)>	12.9	1.7
Completeness [%]	92.0	74.5
Redundancy	7.1	7.3
CC(1/2)	0.999	0.669

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 degree Celsius). Crystallisation was done by the sitting drop method in 96-Well MRC 2-Drop polystyrene Crystallisation Plates (SWISSCI) containing 90 uL of crystallisation solution in the reservoir. Crystals were obtained by mixing 0.7 uL of crystallisation solution with 0.7 uL of protein sample at 22.4 mg.ml-1. 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).