4XXS
Crystal structure of BACE1 with a pyrazole-substituted tetrahydropyran thioamidine
X-RAY DIFFRACTION
Crystallization
Crystalization Experiments | ||||
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ID | Method | pH | Temperature | Details |
1 | VAPOR DIFFUSION, HANGING DROP | 6.6 | 291 | BACE1 lacking the pro-segment was concentrated to ~14 mg/mL in 20 mM Tris pH 7.4 and 250 mM NaCl. Crystallization was carried out by the vapor diffusion method against 200 mM sodium citrate tribasic dihydrate, 22% PEG 5K monomethyl ether and 200 mM ammonium iodide. |
Crystal Properties | |
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Matthews coefficient | Solvent content |
2.78 | 55.7 |
Crystal Data
Unit Cell | |
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Length ( Å ) | Angle ( ˚ ) |
a = 102.35 | α = 90 |
b = 102.35 | β = 90 |
c = 170.55 | γ = 120 |
Symmetry | |
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Space Group | P 61 2 2 |
Diffraction
Diffraction Experiment | ||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
ID # | Crystal ID | Scattering Type | Data Collection Temperature | Detector | Detector Type | Details | Collection Date | Monochromator | Protocol | |||||
1 | 1 | x-ray | 83 | PIXEL | DECTRIS PILATUS 6M | 2012-03-29 | M | SINGLE WAVELENGTH |
Radiation Source | |||||
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ID # | Source | Type | Wavelength List | Synchrotron Site | Beamline |
1 | SYNCHROTRON | APS BEAMLINE 17-ID | 1.0 | APS | 17-ID |
Data Collection
Overall | |||||||||||||||||||
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ID # | Resolution (High) | Resolution (Low) | Percent Possible (Observed) | R Merge I (Observed) | Net I Over Average Sigma (I) | Redundancy | Number Reflections (All) | Number Reflections (Observed) | Observed Criterion Sigma (F) | Observed Criterion Sigma (I) | B (Isotropic) From Wilson Plot | ||||||||
1 | 1.86 | 50 | 99.8 | 0.121 | 4.9 | 17.2 | 44909 | 44.2 |
Highest Resolution Shell | |||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
ID # | Resolution (High) | Resolution (Low) | Percent Possible (All) | Percent Possible (Observed) | Mean I Over Sigma (Observed) | Redundancy | Number Unique Reflections (All) | ||||||||||||
1 | 1.86 | 1.89 | 96.6 | 7.5 | 2132 |
Refinement
Statistics | |||||||||||||||||||
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Diffraction ID | Structure Solution Method | Cross Validation method | Resolution (High) | Resolution (Low) | Number Reflections (Observed) | Number Reflections (R-Free) | Percent Reflections (Observed) | R-Factor (Observed) | R-Work | R-Free | R-Free Selection Details | Mean Isotropic B | |||||||
X-RAY DIFFRACTION | THROUGHOUT | 1.86 | 27.23 | 44821 | 2255 | 99.68 | 0.1831 | 0.1818 | 0.2076 | RANDOM | 50.02 |
Temperature Factor Modeling | ||||||
---|---|---|---|---|---|---|
Anisotropic B[1][1] | Anisotropic B[2][2] | Anisotropic B[3][3] | ||||
4.5971 | 4.5971 | -9.1941 |
RMS Deviations | |
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Key | Refinement Restraint Deviation |
t_other_torsion | 16.47 |
t_omega_torsion | 4.01 |
t_angle_deg | 1.08 |
t_bond_d | 0.01 |
t_dihedral_angle_d | |
t_trig_c_planes | |
t_gen_planes | |
t_it | |
t_nbd | |
t_improper_torsion |
Non-Hydrogen Atoms Used in Refinement | |
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Non-Hydrogen Atoms | Number |
Protein Atoms | 2941 |
Nucleic Acid Atoms | |
Solvent Atoms | 299 |
Heterogen Atoms | 51 |
Software
Software | |
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Software Name | Purpose |
HKL-2000 | data reduction |
BUSTER-TNT | refinement |
PDB_EXTRACT | data extraction |
HKL-2000 | data scaling |
BUSTER-TNT | phasing |