6FS6

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

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE MASSIF-3
Synchrotron site	ESRF
Beamline	MASSIF-3
Temperature [K]	100
Detector technology	PIXEL
Collection date	2017-11-23
Detector	DECTRIS EIGER R 4M
Wavelength(s)	0.9677
Spacegroup name	P 21 21 2
Unit cell lengths	135.180, 75.690, 121.590
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	90.401 - 2.291
R-factor	0.1953
Rwork	0.193
R-free	0.23060
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	PDB:4AWK
RMSD bond length	0.004
RMSD bond angle	0.847
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]	90.401	2.340
High resolution limit [Å]	2.290	2.290
Rmerge		0.908
Number of reflections	59550	4199
<I/σ(I)>	14.8	2.2
Completeness [%]	99.9	100
Redundancy	6.9	7.2
CC(1/2)	0.999	0.770

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING 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 0.3 M (NH4)2SO4, 0.1 M ADA pH 6.5, 28% (w/v) PEG8000