3LON

HCV NS3-4a protease domain with ketoamide inhibitor narlaprevir

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RU200
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2005-04-15
Detector	RIGAKU RAXIS IV
Wavelength(s)	1.5418
Spacegroup name	H 3 2
Unit cell lengths	224.392, 224.392, 75.331
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	8.000 - 2.200
Rwork	0.204
R-free	0.26900
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	208M
RMSD bond length	0.009
RMSD bond angle	1.942
Data reduction software	HKL-2000
Data scaling software	SCALEPACK
Phasing software	X-PLOR
Refinement software	X-PLOR (98.1)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	2.240
High resolution limit [Å]	2.200	2.200
Rmerge	0.045	0.633
Number of reflections	32304
<I/σ(I)>	24.9	1.26
Completeness [%]	88.0	24.8
Redundancy	9.2

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.6	277	Crystallization was performed by the vapor diffusion method using hanging drops (4 L protein solution mixed with 4 L (0.75 - 1.00) M NaCl - 0.1 M MES - 0.1 M Na/K PO4, pH 5.6 - 6.2) suspended over 1 mL reservoir solutions of (1.25 - 1.50) M NaCl - 0.1 M MES - 0.1 M Na/K PO4 - 5 mM -mercaptoethanol, pH 5.6-6.2. The trays were set at 4C for 5-7 days to control nucleation, followed by incubation for 3 weeks at 12C to maximize crystal growth., VAPOR DIFFUSION, HANGING DROP, temperature 277K