3R7R

Structure-based design of thienobenzoxepin inhibitors of PI3-Kinase

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	2007-05-17
Detector	MAR
Wavelength(s)	1.0
Spacegroup name	C 1 2 1
Unit cell lengths	143.792, 67.868, 106.933
Unit cell angles	90.00, 95.40, 90.00

Refinement procedure

Resolution	19.927 - 2.900
R-factor	0.2094
Rwork	0.207
R-free	0.25310
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3e8x
RMSD bond length	0.011
RMSD bond angle	1.562
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	PHENIX (dev_806)

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