6FS7

Influenza A/California/04/2009 (pH1N1) endonuclease with I38T mutation with bound inhibitor, baloxavir acid (BXA)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE MASSIF-1
Synchrotron site	ESRF
Beamline	MASSIF-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2017-10-18
Detector	DECTRIS PILATUS3 2M
Wavelength(s)	0.966
Spacegroup name	P 21 21 2
Unit cell lengths	135.680, 75.560, 121.800
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	90.637 - 1.960
R-factor	0.189
Rwork	0.188
R-free	0.21140
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	PDB:4AWK
RMSD bond length	0.004
RMSD bond angle	0.799
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	PHENIX ((1.12_2829: ???))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	90.637	2.010
High resolution limit [Å]	1.960	1.960
Rmerge		0.596
Number of reflections	94254	6540
<I/σ(I)>	17.4	2.2
Completeness [%]	99.4	99.7
Redundancy	4.1	4
CC(1/2)	0.994	0.767

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	6.5	293	Protein, at 15-17 mg/ml, was incubated with 10-fold molar excess of BXA for 30 min at RT, mixtures were centrifuged at RT for 5 minutes at 12000 g, and soluble fraction was used for crystallization trials (final protein concentration 8-10 mg/ml). Mother liquor was 0.2 M (NH4)2SO4, 0.1 M Na(CH3)2AsO2 pH 6.5, 30% (w/v) PEG8000