6NCJ

Structure of HIV-1 Integrase with potent 5,6,7,8-Tetrahydro-1,6-naphthyridine Derivatives Allosteric Site Inhibitors

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	2012-11-20
Detector	DECTRIS PILATUS 6M
Wavelength(s)	1.00000
Spacegroup name	P 31 2 1
Unit cell lengths	72.290, 72.290, 64.790
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	31.570 - 2.000
R-factor	0.196
Rwork	0.194
R-free	0.24000
RMSD bond length	0.010
RMSD bond angle	1.070
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	PHENIX
Refinement software	BUSTER

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	44.990	2.030
High resolution limit [Å]	2.000	2.000
Rmerge	0.034	0.916
Rmeas	0.033	0.974
Rpim	0.011	0.329
Number of reflections	13589	668
<I/σ(I)>	36.1	2.14
Completeness [%]	100.0	100
Redundancy	9.6	8.6
CC(1/2)		0.785

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		293	The optimized conditions consisted of a reservoir solution with 1.8 - 2.2 M ammonium sulfate and 100 mM sodium acetate pH 4.6 - 5.5. Drops were formed from 0.3 mL of the protein solution and 0.3 mL of the reservoir solution (total initial volume of 0.6 mL), mixed, and placed at 20C to equilibrate.