4EZL

Potent and Selective Inhibitors of PI3K-delta: Obtaining Isoform Selectivity from the Affinity Pocket and Tryptophan Shelf

Experimental procedure

Experimental method	SINGLE
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.1
Synchrotron site	ALS
Beamline	5.0.1
Detector technology	CCD
Collection date	2011-10-26
Detector	ADSC QUANTUM 210
Wavelength(s)	1.0
Spacegroup name	C 1 2 1
Unit cell lengths	141.331, 67.194, 106.558
Unit cell angles	90.00, 96.10, 90.00

Refinement procedure

Resolution	31.140 - 2.940
R-factor	0.245
Rwork	0.244
R-free	0.27100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1e8x
RMSD bond length	0.008
RMSD bond angle	1.531
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	PHASER (2.3.0)
Refinement software	PHENIX (1.7.2_869)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	3.110
High resolution limit [Å]	2.935	6.460	2.935
Rmerge	0.086	0.050	0.475
Number of reflections	20407
<I/σ(I)>	10.1
Completeness [%]	99.5	99	99.8
Redundancy	3.6	3.5	3.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8.5	289	PEG 3350, 0.2M NH4SO4, 0.1M Tris-HCl 8.5, vapor diffusion, hanging drop, temperature 289K