4XBB

1.85A resolution structure of Norovirus 3CL protease complex with a covalently bound dipeptidyl inhibitor diethyl [(1R,2S)-2-[(N-{[(3-chlorobenzyl)oxy]carbonyl}-3-cyclohexyl-L-alanyl)amino]-1-hydroxy-3-(2-oxo-2H-pyrrol-3-yl)propyl]phosphonate

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	100
Detector technology	PIXEL
Collection date	2014-04-17
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.0000
Spacegroup name	P 65 2 2
Unit cell lengths	124.171, 124.171, 49.969
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	45.316 - 1.850
R-factor	0.1641
Rwork	0.163
R-free	0.19650
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3ur9
RMSD bond length	0.009
RMSD bond angle	1.229
Data scaling software	Aimless (0.2.17)
Phasing software	PHASER (2.5.6)
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.320	45.320	1.890
High resolution limit [Å]	1.850	9.060	1.850
Rmerge	0.197	0.051	1.505
Total number of observations	384657	3510	22129
Number of reflections	19899
<I/σ(I)>	14.9	46.1	2.4
Completeness [%]	100.0	99.5	100
Redundancy	19.3	16	18.5
CC(1/2)	0.998	0.999	0.763

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	7.5	293	20% (w/v) PEG 5000 MME, 100 mM Tris, 200 mM ammonium sulfate