8ATL

Discovery of IRAK4 Inhibitor 23


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP4.92930.1M sodium acetate buffer pH 4.9, 2.13-2.145M sodium malonate
Crystal Properties
Matthews coefficientSolvent content
2.8256.4

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 87.864α = 90
b = 118.789β = 90
c = 138.136γ = 90
Symmetry
Space GroupI 2 2 2

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100PIXELDECTRIS PILATUS 6M2013-11-13MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONBESSY BEAMLINE 14.10.9184BESSY14.1

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)Rrim I (All)CC (Half)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
12.4646.35499.80.0740.99917.35.5146185
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)Rrim I (All)CC (Half)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
12.462.61000.4910.926

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodStarting modelResolution (High)Resolution (Low)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-Factor (All)R-WorkR-FreeMean Isotropic B
X-RAY DIFFRACTIONMOLECULAR REPLACEMENTFREE R-VALUEin house model2.46446.35426316131699.3920.2010.19880.242956.279
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]
-0.3373.653-3.316
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.827
r_dihedral_angle_4_deg26.04
r_dihedral_angle_3_deg17.607
r_lrange_other11.908
r_lrange_it11.906
r_scangle_other9.523
r_scangle_it9.522
r_mcangle_it8.075
r_mcangle_other8.074
r_scbond_other6.124
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.827
r_dihedral_angle_4_deg26.04
r_dihedral_angle_3_deg17.607
r_lrange_other11.908
r_lrange_it11.906
r_scangle_other9.523
r_scangle_it9.522
r_mcangle_it8.075
r_mcangle_other8.074
r_scbond_other6.124
r_scbond_it6.123
r_dihedral_angle_1_deg5.699
r_mcbond_it5.291
r_mcbond_other5.289
r_angle_refined_deg1.274
r_angle_other_deg1.091
r_symmetry_xyhbond_nbd_refined0.22
r_nbd_refined0.168
r_symmetry_nbd_other0.168
r_nbd_other0.162
r_nbtor_refined0.15
r_symmetry_nbd_refined0.112
r_xyhbond_nbd_refined0.107
r_xyhbond_nbd_other0.103
r_symmetry_nbtor_other0.075
r_chiral_restr0.041
r_bond_refined_d0.003
r_gen_planes_refined0.003
r_bond_other_d0.001
r_gen_planes_other0.001
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms4354
Nucleic Acid Atoms
Solvent Atoms70
Heterogen Atoms70

Software

Software
Software NamePurpose
REFMACrefinement
XDSdata reduction
XSCALEdata scaling
MOLREPphasing