3NZU

Structure-based Optimization of Pyrazolo -Pyrimidine and -Pyridine Inhibitors of PI3-Kinase

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	2008-04-10
Detector	ADSC QUANTUM 315
Wavelength(s)	1.0
Spacegroup name	C 1 2 1
Unit cell lengths	144.004, 67.677, 106.362
Unit cell angles	90.00, 95.52, 90.00

Refinement procedure

Resolution	19.880 - 2.600
R-factor	0.2143
Rwork	0.213
R-free	0.24050
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.002
RMSD bond angle	0.473
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	PHASER (2.1.4)
Refinement software	PHENIX (dev_392)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.690
High resolution limit [Å]	2.600	5.600	2.600
Rmerge	0.049	0.028	0.592
Number of reflections	31733
<I/σ(I)>	17.7
Completeness [%]	99.9	99.1	100
Redundancy	3.7	3.6	3.8

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