4PZW
Synthesis, Characterization and PK/PD Studies of a Series of Spirocyclic Pyranochromene BACE1 Inhibitors
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | ROTATING ANODE |
Source details | RIGAKU FR-E SUPERBRIGHT |
Temperature [K] | 100 |
Detector technology | IMAGE PLATE |
Collection date | 2011-09-20 |
Detector | RIGAKU RAXIS IV++ |
Wavelength(s) | 1.5418 |
Spacegroup name | C 2 2 21 |
Unit cell lengths | 75.170, 103.940, 99.730 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 29.130 - 1.800 |
R-factor | 0.20367 |
Rwork | 0.202 |
R-free | 0.23124 |
Structure solution method | MOLECULAR REPLACEMENT |
RMSD bond length | 0.006 |
RMSD bond angle | 1.136 |
Data reduction software | MOSFLM |
Data scaling software | SCALA |
Phasing software | MOLREP |
Refinement software | REFMAC (5.8.0049) |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 30.000 | 1.900 |
High resolution limit [Å] | 1.800 | 1.800 |
Rmerge | 0.058 | 0.111 |
Number of reflections | 36157 | |
<I/σ(I)> | 13.9 | 7.9 |
Completeness [%] | 99.0 | 93 |
Redundancy | 6.6 | 3.8 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 4.5 | 300 | 16% PEG3K, 0.1M NaAcetate, 5% DMSO, VAPOR DIFFUSION, HANGING DROP, temperature 300K, pH 4.5 |