2Q15

Structure of BACE complexed to compound 3a


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, SITTING DROP6.629322.5% (w/v) PEG 5000 monomethylethyl (MME), 200 mM sodium citrate, 200 mM ammonium iodide, pH 6.6, VAPOR DIFFUSION, SITTING DROP, temperature 293K
Crystal Properties
Matthews coefficientSolvent content
2.9958.83

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 102.347α = 90
b = 102.347β = 90
c = 169.715γ = 120
Symmetry
Space GroupP 61 2 2

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONESRF BEAMLINE ID14-2ESRFID14-2

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Sym 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
12.429.5499.810.0935.720102
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R-Sym I (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
2.40.39

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 DIFFRACTIONMOLECULAR REPLACEMENTTHROUGHOUT2.429.5420102109199.810.256050.25150.3438RANDOM47.498
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]
0.130.070.13-0.2
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_1_deg9.684
r_scangle_it7.157
r_mcangle_it5.984
r_scbond_it5.399
r_mcbond_it4.357
r_angle_refined_deg2.105
r_angle_other_deg1.073
r_xyhbond_nbd_refined0.307
r_nbd_other0.25
r_nbd_refined0.243
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_1_deg9.684
r_scangle_it7.157
r_mcangle_it5.984
r_scbond_it5.399
r_mcbond_it4.357
r_angle_refined_deg2.105
r_angle_other_deg1.073
r_xyhbond_nbd_refined0.307
r_nbd_other0.25
r_nbd_refined0.243
r_symmetry_vdw_other0.241
r_symmetry_vdw_refined0.199
r_symmetry_hbond_refined0.16
r_chiral_restr0.117
r_nbtor_other0.096
r_bond_refined_d0.024
r_gen_planes_refined0.008
r_gen_planes_other0.003
r_bond_other_d0.002
r_dihedral_angle_2_deg
r_dihedral_angle_3_deg
r_dihedral_angle_4_deg
r_nbtor_refined
r_xyhbond_nbd_other
r_metal_ion_refined
r_metal_ion_other
r_symmetry_hbond_other
r_symmetry_metal_ion_refined
r_symmetry_metal_ion_other
r_mcbond_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms3023
Nucleic Acid Atoms
Solvent Atoms157
Heterogen Atoms37

Software

Software
Software NamePurpose
REFMACrefinement