2FM2

HCV NS3-4A protease domain complexed with a ketoamide inhibitor, SCH446211

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RUH3R
Temperature [K]	95
Detector technology	IMAGE PLATE
Collection date	2005-04-14
Detector	RIGAKU RAXIS IV
Wavelength(s)	1.5418
Spacegroup name	H 3 2
Unit cell lengths	224.909, 224.909, 75.402
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	8.000 - 2.700
R-factor	0.189
Rwork	0.185
R-free	0.26000
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	HCV NS3(139A)/4A protease domain structure
RMSD bond length	0.008
RMSD bond angle	1.930
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	2.780
High resolution limit [Å]	2.700	2.700
Number of reflections	19511
<I/σ(I)>	13.6	3
Completeness [%]	98.1	84.7
Redundancy	4	2.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.7	285	Crystallization was performed by the vapor diffusion method using hanging drops (4 uL protein solution mixed with 4 uL (0.75 - 1.00)M NaCl - 0.1M MES - 0.1M Na/K PO4, pH 5.6 - 5.8) suspended over 1mL reservoir solutions of (1.25 - 1.50)M NaCl - 0.1M MES - 0.1M Na/K PO4 - 5mM-mercaptoethanol, pH 5.6-5.8. 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. , pH 5.7, VAPOR DIFFUSION, HANGING DROP, temperature 285K