4EZK

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 5.0.2
Synchrotron site	ALS
Beamline	5.0.2
Detector technology	CCD
Collection date	2011-12-01
Detector	ADSC QUANTUM 315
Wavelength(s)	1.0
Spacegroup name	C 1 2 1
Unit cell lengths	140.730, 67.190, 106.020
Unit cell angles	90.00, 96.76, 90.00

Refinement procedure

Resolution	34.392 - 2.803
R-factor	0.2437
Rwork	0.243
R-free	0.25330
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1e8x
RMSD bond length	0.009
RMSD bond angle	1.463
Data scaling software	SCALA (3.3.20)
Phasing software	PHASER
Refinement software	PHENIX (1.8_1066)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	34.392	34.392	2.950
High resolution limit [Å]	2.800	8.860	2.800
Rmerge		0.018	0.331
<I/σ(I)>	22.5	32	2.1
Completeness [%]	95.6	96.8	91
Redundancy	3.2	3.4	3.2

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