3R7Q

Structure-based design of thienobenzoxepin inhibitors of PI3- kinase

Experimental procedure

Experimental method	SINGLE
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL9-2
Synchrotron site	SSRL
Beamline	BL9-2
Detector technology	CCD
Collection date	2007-05-17
Detector	MAR
Wavelength(s)	1.0
Spacegroup name	C 1 2 1
Unit cell lengths	141.782, 67.494, 105.892
Unit cell angles	90.00, 96.43, 90.00

Refinement procedure

Resolution	19.927 - 2.500
R-factor	0.2189
Rwork	0.216
R-free	0.26860
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1e8x
RMSD bond length	0.013
RMSD bond angle	1.762
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	PHENIX (dev_798)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.590
High resolution limit [Å]	2.500	5.380	2.500
Rmerge	0.042	0.023	0.549
Number of reflections	34114
<I/σ(I)>	15.7
Completeness [%]	98.6	97.1	94.6
Redundancy	2.8	2.7	2.4

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
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