3ZSY

Small molecule inhibitors of the LEDGF site of HIV type 1 integrase identified by fragment screening and structure based drug design

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	AUSTRALIAN SYNCHROTRON BEAMLINE MX1
Synchrotron site	Australian Synchrotron
Beamline	MX1
Temperature [K]	100
Detector technology	CCD
Collection date	2009-07-29
Detector	ADSC QUANTUM 210r
Spacegroup name	P 31
Unit cell lengths	70.692, 70.692, 66.889
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	35.360 - 2.200
R-factor	0.1828
Rwork	0.181
R-free	0.22175
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3nf7
RMSD bond length	0.015
RMSD bond angle	1.612
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	PHASER
Refinement software	REFMAC (5.2.0019)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	45.200	2.320
High resolution limit [Å]	2.200	2.200
Rmerge	0.130	0.630
Number of reflections	19005
<I/σ(I)>	13.1	2.5
Completeness [%]	100.0	100
Redundancy	5.5	5.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1		5.5		THE PROTEIN WAS CONCENTRATED TO 5.5MG/ML IN 40 MM TRIS PH 8.0, 250 MM NACL, 30 MM MGCL2, 5 MM DTT AND SET UP IN A 1:1 RATIO WITH 1.6 TO 2.0 M AMMONIUM SULFATE, 100 MM SODIUM ACETATE BUFFER PH 5.0 TO 5.5.