9OES

HalA with lysine, succinate, chloride, and vanadium(IV)-oxo at pH 4.2

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 8.3.1
Synchrotron site	ALS
Beamline	8.3.1
Temperature [K]	90
Detector technology	PIXEL
Collection date	2021-12-03
Detector	DECTRIS PILATUS3 S 6M
Wavelength(s)	1.11583
Spacegroup name	H 3
Unit cell lengths	146.950, 146.950, 287.970
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	95.350 - 1.930
R-factor	0.1766
Rwork	0.174
R-free	0.21630
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.007
RMSD bond angle	0.813
Data reduction software	XDS (Feb 5, 2021)
Data scaling software	Aimless (0.7.9)
Phasing software	PHASER (2.8.3)
Refinement software	PHENIX (1.21rc1_5156)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	95.990	1.960
High resolution limit [Å]	1.930	1.930
Rmerge	0.361	5.306
Rmeas	0.368	5.528
Rpim	0.070	1.517
Number of reflections	173594	201303
<I/σ(I)>	13.5	0.7
Completeness [%]	99.6	94.3
Redundancy	53.12	24.77
CC(1/2)	0.999	0.536

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		291	HalA crystals were obtained by the sitting drop vapor diffusion method by combining equal volumes of protein solution (HalA (15 mg/ml), lysine (50 mM, pH 7), sodium succinate (20 mM, pH 7), sodium chloride (100 mM) and vanadium(IV) oxide sulfate hydrate (1 mM, dissolved in 2.5 mM H2SO4)) and reservoir solution (sodium phosphate dibasic/citric acid (100 mM), 40% (w/v) PEG 300, pH 4.2)