3LPB

Crystal structure of Jak2 complexed with a potent 2,8-diaryl-quinoxaline inhibitor


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP6.229830% PEG4000, 0.1M AMMONIUM SULFATE, 0.1M NA CITRATE, pH 6.2, VAPOR DIFFUSION, HANGING DROP, temperature 298K
Crystal Properties
Matthews coefficientSolvent content
3.2161.71

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 112.39α = 90
b = 112.39β = 90
c = 70.651γ = 90
Symmetry
Space GroupP 41

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMARMOSAIC 225 mm CCDSAGITALLY FOCUSED SI(III)2006-10-21MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSLS BEAMLINE X10SA0.99990SLSX10SA

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
1279.4998.80.0515.063.325898136.6
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)
22.0690.10.3473.32.874533

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 REPLACEMENTTHROUGHOUT2b7a279.4756062292098.840.177910.176410.20674RANDOM33.946
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]
0.690.69-1.39
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg39.362
r_dihedral_angle_4_deg20.364
r_dihedral_angle_3_deg13.763
r_scangle_it6.822
r_dihedral_angle_1_deg5.552
r_scbond_it4.418
r_mcangle_it2.904
r_mcbond_it1.7
r_angle_refined_deg1.411
r_chiral_restr0.093
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg39.362
r_dihedral_angle_4_deg20.364
r_dihedral_angle_3_deg13.763
r_scangle_it6.822
r_dihedral_angle_1_deg5.552
r_scbond_it4.418
r_mcangle_it2.904
r_mcbond_it1.7
r_angle_refined_deg1.411
r_chiral_restr0.093
r_bond_refined_d0.014
r_gen_planes_refined0.007
r_bond_other_d
r_angle_other_deg
r_gen_planes_other
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_mcbond_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms4556
Nucleic Acid Atoms
Solvent Atoms310
Heterogen Atoms66

Software

Software
Software NamePurpose
PHASERphasing
REFMACrefinement
XDSdata reduction
XSCALEdata scaling