3G90

JNK-3 bound to (Z)-5-fluoro-1-((6-fluoro-4H-benzo[d][1,3]dioxin-8-yl)methyl)-3-(hydroxyimino)indolin-2-one


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP7.529818-20% (v/v) polyethylene glycol monomethyl ether (average Mr = 550), 10% (v/v) ethylene glycol, 20 mM beta-mercaptoethanol, 100 mM HEPES, pH 7.5, VAPOR DIFFUSION, HANGING DROP, temperature 298K
Crystal Properties
Matthews coefficientSolvent content
2.2846.14

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 49.655α = 90
b = 72.289β = 90
c = 107.189γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100IMAGE PLATERIGAKU RAXIS IV++1998-05-01MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1ROTATING ANODERIGAKU RUH3R1.5418

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
12.46096.90.06717.22.61524312
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R Merge I (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
12.42.4794.80.374

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodResolution (High)Resolution (Low)Number Reflections (All)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-Factor (Observed)R-WorkR-FreeR-Free Selection DetailsMean Isotropic B
X-RAY DIFFRACTIONFOURIER SYNTHESISTHROUGHOUT2.434.26148511485174899.480.218050.21550.2664RANDOM41.315
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]
3.78-2.49-1.29
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg39.387
r_dihedral_angle_4_deg18.551
r_dihedral_angle_3_deg17.742
r_dihedral_angle_1_deg5.778
r_scangle_it1.807
r_angle_refined_deg1.233
r_scbond_it1.155
r_mcangle_it0.866
r_mcbond_it0.534
r_nbtor_refined0.301
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg39.387
r_dihedral_angle_4_deg18.551
r_dihedral_angle_3_deg17.742
r_dihedral_angle_1_deg5.778
r_scangle_it1.807
r_angle_refined_deg1.233
r_scbond_it1.155
r_mcangle_it0.866
r_mcbond_it0.534
r_nbtor_refined0.301
r_symmetry_vdw_refined0.228
r_nbd_refined0.196
r_symmetry_hbond_refined0.168
r_xyhbond_nbd_refined0.159
r_chiral_restr0.081
r_bond_refined_d0.01
r_gen_planes_refined0.003
r_bond_other_d
r_angle_other_deg
r_gen_planes_other
r_nbd_other
r_nbtor_other
r_xyhbond_nbd_other
r_metal_ion_refined
r_metal_ion_other
r_symmetry_vdw_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 Atoms2800
Nucleic Acid Atoms
Solvent Atoms62
Heterogen Atoms25

Software

Software
Software NamePurpose
CrystalCleardata collection
REFMACrefinement
DENZOdata reduction
SCALEPACKdata scaling