6OTG

HIV-1 protease triple mutants V32I, I47V, V82I with GRL-011-11A (a methylamine bis-Tetrahydrofuran P2-Ligand, sulfonamide isostere derivate)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 22-BM
Synchrotron site	APS
Beamline	22-BM
Temperature [K]	100
Detector technology	CCD
Collection date	2017-06-28
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	1.0
Spacegroup name	P 21 21 2
Unit cell lengths	58.574, 86.517, 46.322
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	33.520 - 1.500
R-factor	0.13356
Rwork	0.132
R-free	0.17132
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3nu3
RMSD bond length	0.019
RMSD bond angle	2.242
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER (2.7.17)
Refinement software	REFMAC (5.8.0238)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	1.550
High resolution limit [Å]	1.500	1.500
Rmerge	0.059	0.493
Rmeas	0.064	0.569
Rpim	0.024	0.278
Number of reflections	37188	2865
<I/σ(I)>	26.6	3.1
Completeness [%]	96.8	76.4
Redundancy	6.7	4.1
CC(1/2)	0.998	0.803

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	4.6	298	The protein (about 5 mg/mL) was preincubated with the inhibitor (dissolved in dimethylsulfoxide) at a molar ratio of 1:5. Crystals were grown from 0.1 m sodium acetate buffer, pH 4.6 and 2M NaCl as precipitant. Crystals were cryo-cooled in liquid nitrogen after soaking in 30% glycerol to prevent freezing.