5B18

Crystal Structure of a Darunavir Resistant HIV-1 Protease

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SPRING-8 BEAMLINE BL38B1
Synchrotron site	SPring-8
Beamline	BL38B1
Temperature [K]	100
Detector technology	CCD
Collection date	2011-11-11
Detector	ADSC QUANTUM 4r
Wavelength(s)	1.0
Spacegroup name	P 1
Unit cell lengths	37.149, 48.699, 54.151
Unit cell angles	89.90, 73.98, 86.69

Refinement procedure

Resolution	50.000 - 1.800
R-factor	0.1951
Rwork	0.193
R-free	0.24420
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1kj7
RMSD bond length	0.019
RMSD bond angle	2.016
Data reduction software	HKL-2000
Data scaling software	SCALEPACK
Phasing software	MOLREP
Refinement software	REFMAC (5.6.0117)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.860
High resolution limit [Å]	1.800	3.880	1.800
Rmerge	0.046	0.032	0.233
Total number of observations	62603
Number of reflections	32575
<I/σ(I)>	17
Completeness [%]	96.0	96.6	92.7
Redundancy	1.9	1.9	1.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	4	277	LiCl, Na citrate, PEG 6000, Glycerol, Ethylene glycol