8ATN

Discovery of IRAK4 Inhibitor 38


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, SITTING DROP4.92930.1M sodium acetate buffer pH 4.9, 1.5-1.7M ammonium citrate, 0.02M hexaaminecobalt(III)chloride
Crystal Properties
Matthews coefficientSolvent content
2.7855.92

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 88.194α = 90
b = 118.899β = 90
c = 140.475γ = 90
Symmetry
Space GroupI 2 2 2

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100PIXELDECTRIS EIGER X 16M2021-10-02MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONPETRA III, EMBL c/o DESY BEAMLINE P14 (MX2)0.9763PETRA III, EMBL c/o DESYP14 (MX2)

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
12.1749.8899.90.1190.99913.7713.7539306
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)CC (Half)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
12.172.30.767

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 model2.17149.87539289196599.8980.2420.23840.305977.038
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]
-8.8998.2350.664
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg40.338
r_dihedral_angle_4_deg25.87
r_dihedral_angle_3_deg23.671
r_lrange_it12.842
r_lrange_other12.839
r_scangle_it10.794
r_scangle_other10.792
r_scbond_it7.431
r_scbond_other7.429
r_mcangle_it7.333
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg40.338
r_dihedral_angle_4_deg25.87
r_dihedral_angle_3_deg23.671
r_lrange_it12.842
r_lrange_other12.839
r_scangle_it10.794
r_scangle_other10.792
r_scbond_it7.431
r_scbond_other7.429
r_mcangle_it7.333
r_mcangle_other7.333
r_dihedral_angle_1_deg6.611
r_mcbond_it5.12
r_mcbond_other5.116
r_angle_refined_deg1.767
r_angle_other_deg1.356
r_symmetry_nbd_refined0.632
r_nbd_other0.255
r_nbd_refined0.228
r_symmetry_nbd_other0.221
r_nbtor_refined0.173
r_xyhbond_nbd_refined0.157
r_symmetry_nbtor_other0.088
r_symmetry_xyhbond_nbd_refined0.083
r_chiral_restr0.073
r_symmetry_xyhbond_nbd_other0.031
r_bond_refined_d0.014
r_gen_planes_refined0.01
r_bond_other_d0.005
r_gen_planes_other0.002
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms4451
Nucleic Acid Atoms
Solvent Atoms23
Heterogen Atoms66

Software

Software
Software NamePurpose
REFMACrefinement
XDSdata reduction
XSCALEdata scaling
MOLREPphasing