5M0D

Structure-based evolution of a hybrid steroid series of Autotaxin inhibitors


X-RAY DIFFRACTION

Starting Model(s)

Initial Refinement Model(s)
TypeSourceAccession CodeDetails
experimental modelPDB 2XR9 

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP293PEG3350, NaSCN and NH4I
Crystal Properties
Matthews coefficientSolvent content
2.243.97

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 62.927α = 90
b = 88.012β = 103.1
c = 77.356γ = 90
Symmetry
Space GroupP 1 21 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100PIXELDECTRIS PILATUS 2M2016-05-29MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSLS BEAMLINE X06DA0.9801SLSX06DA

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (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
12.475.3498.341.94.550000

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodStarting modelResolution (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 REPLACEMENTTHROUGHOUT2XR92.475.3430558156899.710.227130.224930.26966RANDOM59.659
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]
-0.581.57-3.342.88
RMS Deviations
KeyRefinement Restraint Deviation
r_sphericity_bonded82.075
r_sphericity_free38.132
r_dihedral_angle_2_deg33.536
r_dihedral_angle_4_deg16.647
r_dihedral_angle_3_deg14.131
r_dihedral_angle_1_deg7.009
r_long_range_B_refined3.597
r_long_range_B_other3.597
r_angle_refined_deg1.377
r_angle_other_deg0.934
RMS Deviations
KeyRefinement Restraint Deviation
r_sphericity_bonded82.075
r_sphericity_free38.132
r_dihedral_angle_2_deg33.536
r_dihedral_angle_4_deg16.647
r_dihedral_angle_3_deg14.131
r_dihedral_angle_1_deg7.009
r_long_range_B_refined3.597
r_long_range_B_other3.597
r_angle_refined_deg1.377
r_angle_other_deg0.934
r_mcangle_it0.608
r_mcangle_other0.608
r_scangle_other0.388
r_mcbond_it0.323
r_mcbond_other0.32
r_scbond_it0.217
r_scbond_other0.215
r_chiral_restr0.075
r_bond_refined_d0.008
r_gen_planes_refined0.006
r_bond_other_d0.002
r_gen_planes_other0.001
r_nbd_refined
r_nbd_other
r_nbtor_refined
r_nbtor_other
r_xyhbond_nbd_refined
r_xyhbond_nbd_other
r_metal_ion_refined
r_metal_ion_other
r_symmetry_vdw_refined
r_symmetry_vdw_other
r_symmetry_hbond_refined
r_symmetry_hbond_other
r_symmetry_metal_ion_refined
r_symmetry_metal_ion_other
r_scangle_it
r_rigid_bond_restr
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms6251
Nucleic Acid Atoms
Solvent Atoms19
Heterogen Atoms181

Software

Software
Software NamePurpose
REFMACrefinement
XDSdata reduction
Aimlessdata scaling
PHASERphasing