4L7G

Diethylaminosulfur Trifluoride-Mediated Intramolecular Cyclization of 2-hydroxy-benzylureas to Fused Bicyclic Aminooxazoline Compounds and Evaluation of Their Biochemical Activity Against Beta-Secretase-1 (BACE1)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 21-ID-F
Synchrotron site	APS
Beamline	21-ID-F
Temperature [K]	93
Detector technology	CCD
Collection date	2010-11-05
Detector	RAYONIX MX-225
Wavelength(s)	0.97872
Spacegroup name	C 1 2 1
Unit cell lengths	72.664, 104.471, 50.076
Unit cell angles	90.00, 94.82, 90.00

Refinement procedure

Resolution	16.633 - 1.380
R-factor	0.1563
Rwork	0.154
R-free	0.19160
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1fkn
RMSD bond length	0.006
RMSD bond angle	1.121
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	PHASER
Refinement software	PHENIX ((phenix.refine: 1.6.4_486))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	50.000	1.430
High resolution limit [Å]	1.380	1.380
Number of reflections	75939
Completeness [%]	99.6	99.8
Redundancy	3.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	4.9	292	12% PEG 3350 and 0.1M NaOAc, pH 4.9, VAPOR DIFFUSION, SITTING DROP, temperature 292K