2XA4

Inhibitors of Jak2 Kinase domain


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP6293HANGING DROP 20 DEG C. 1.5UL PROTEIN PLUS 1UL WELL PROTEIN: 8.7MG/ML IN 20MM TRIS/HCL PH 8.5, 100MM NACL, 1MM DTT WELL: 28% W/V PEG3350, 200MM AMMONIUM ACETATE, 100MM SODIUM CITRATE PH 6.0
Crystal Properties
Matthews coefficientSolvent content
2.7755.66

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 43.854α = 90
b = 126.741β = 97.04
c = 134.342γ = 90
Symmetry
Space GroupC 1 2 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC CCDMIRRORS2007-03-07MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONESRF BEAMLINE ID23-2ESRFID23-2

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
11.833.3393.40.078.023.0443209222.815
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)
12.042.0987.20.41.862.92

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodResolution (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 REPLACEMENTTHROUGHOUT2.0433.3341003219293.340.199620.197190.24456RANDOM26.225
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]
2.341.160.02-2.07
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg38.009
r_dihedral_angle_3_deg16.019
r_dihedral_angle_4_deg15.89
r_dihedral_angle_1_deg5.927
r_scangle_it2.926
r_scbond_it1.767
r_angle_refined_deg1.342
r_mcangle_it1.322
r_angle_other_deg0.856
r_mcbond_it0.7
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg38.009
r_dihedral_angle_3_deg16.019
r_dihedral_angle_4_deg15.89
r_dihedral_angle_1_deg5.927
r_scangle_it2.926
r_scbond_it1.767
r_angle_refined_deg1.342
r_mcangle_it1.322
r_angle_other_deg0.856
r_mcbond_it0.7
r_mcbond_other0.122
r_chiral_restr0.073
r_bond_refined_d0.01
r_gen_planes_refined0.005
r_bond_other_d0.001
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_mcangle_other
r_scbond_other
r_scangle_other
r_long_range_B_refined
r_long_range_B_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms4511
Nucleic Acid Atoms
Solvent Atoms308
Heterogen Atoms48

Software

Software
Software NamePurpose
REFMACrefinement
MOSFLMdata reduction
SCALAdata scaling
AMoREphasing