3ZSQ

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 MX2
Synchrotron site	Australian Synchrotron
Beamline	MX2
Temperature [K]	100
Detector technology	CCD
Collection date	2009-10-31
Detector	ADSC QUANTUM 315
Spacegroup name	P 31
Unit cell lengths	70.965, 70.965, 67.685
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	61.460 - 1.700
R-factor	0.16292
Rwork	0.161
R-free	0.19991
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3nf7
RMSD bond length	0.029
RMSD bond angle	2.372
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	PHASER
Refinement software	REFMAC (5.5.0102)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	67.700	1.790
High resolution limit [Å]	1.700	1.700
Rmerge	0.100	0.290
Number of reflections	41971
<I/σ(I)>	11.3	4.8
Completeness [%]	99.9	100
Redundancy	5.6	5.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1		5.5		THE PROTEIN WAS CONCENTRATED TO 5.5 MG/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.