4L7H
Diethylaminosulfur Trifluoride-Mediated Intramolecular Cyclization of 2-hydroxy-benzylureas to Fused Bicyclic Aminooxazoline Compounds and Evaluation of Their Biochemical Activity Against Beta-Secretase-1 (BACE-1)
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | ALS BEAMLINE 5.0.1 |
Synchrotron site | ALS |
Beamline | 5.0.1 |
Temperature [K] | 93 |
Detector technology | CCD |
Collection date | 2010-11-23 |
Detector | ADSC QUANTUM 315 |
Wavelength(s) | 0.97740 |
Spacegroup name | C 1 2 1 |
Unit cell lengths | 73.062, 104.679, 49.995 |
Unit cell angles | 90.00, 94.97, 90.00 |
Refinement procedure
Resolution | 36.988 - 1.850 |
R-factor | 0.1892 |
Rwork | 0.187 |
R-free | 0.22720 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 1fkn |
RMSD bond length | 0.006 |
RMSD bond angle | 1.158 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Phasing software | PHASER |
Refinement software | PHENIX ((phenix.refine: 1.7.3_928)) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 50.000 | 1.920 |
High resolution limit [Å] | 1.850 | 1.850 |
Number of reflections | 31006 | |
Completeness [%] | 97.0 | 85.2 |
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 |