Experiment: 4XXS

 4XXS

Crystal structure of BACE1 with a pyrazole-substituted tetrahydropyran thioamidine


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP6.6291BACE1 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
Matthews coefficientSolvent content
2.7855.7

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 102.35α = 90
b = 102.35β = 90
c = 170.55γ = 120
Symmetry
Space GroupP 61 2 2

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray83PIXELDECTRIS PILATUS 6M2012-03-29MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONAPS BEAMLINE 17-ID1.0APS17-ID

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Merge I (Observed)Net I Over Average Sigma (I)RedundancyNumber Reflections (All)Number Reflections (Observed)Observed Criterion Sigma (F)Observed Criterion Sigma (I)B (Isotropic) From Wilson Plot
11.865099.80.1214.917.24490944.2
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
11.861.8996.67.52132

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodResolution (High)Resolution (Low)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-Factor (Observed)R-WorkR-FreeR-Free Selection DetailsMean Isotropic B
X-RAY DIFFRACTIONTHROUGHOUT1.8627.2344821225599.680.18310.18180.2076RANDOM50.02
Temperature Factor Modeling
Anisotropic B[1][1]Anisotropic B[1][2]Anisotropic B[1][3]Anisotropic B[2][2]Anisotropic B[2][3]Anisotropic B[3][3]
4.59714.5971-9.1941
RMS Deviations
KeyRefinement Restraint Deviation
t_other_torsion16.47
t_omega_torsion4.01
t_angle_deg1.08
t_bond_d0.01
t_dihedral_angle_d
t_trig_c_planes
t_gen_planes
t_it
t_nbd
t_improper_torsion
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms2941
Nucleic Acid Atoms
Solvent Atoms299
Heterogen Atoms51

Software

Software
Software NamePurpose
HKL-2000data reduction
BUSTER-TNTrefinement
PDB_EXTRACTdata extraction
HKL-2000data scaling
BUSTER-TNTphasing