3FUP

Crystal structures of JAK1 and JAK2 inhibitor complexes


X-RAY DIFFRACTION

Starting Model(s)

Initial Refinement Model(s)
TypeSourceAccession CodeDetails
experimental modelPDB 2B7APDB ENTRY 2B7A

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP28018% PEG 8000, 100 mM Cacodylate, pH 6.5/6.7, 100 mM magnesium acetate, 100 mM KCl , VAPOR DIFFUSION, HANGING DROP, temperature 280K
Crystal Properties
Matthews coefficientSolvent content
3.160.35

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 110.491α = 90
b = 110.491β = 90
c = 70.317γ = 90
Symmetry
Space GroupP 41

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100IMAGE PLATERIGAKU RAXIS IVmirrors2005-04-13MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1ROTATING ANODERIGAKU RUH2R1.5418

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
12.4110.430.09313.3529833
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)
2.42.490.531

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 REPLACEMENTTHROUGHOUTPDB ENTRY 2B7A2.4110.4329833160194.330.181590.178060.24966RANDOM44.983
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]
0.710.71-1.43
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg40.132
r_dihedral_angle_4_deg22.147
r_dihedral_angle_3_deg18.421
r_scangle_it10.542
r_scbond_it7.553
r_dihedral_angle_1_deg6.626
r_mcangle_it4.559
r_mcbond_it2.894
r_angle_refined_deg1.823
r_nbtor_refined0.321
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg40.132
r_dihedral_angle_4_deg22.147
r_dihedral_angle_3_deg18.421
r_scangle_it10.542
r_scbond_it7.553
r_dihedral_angle_1_deg6.626
r_mcangle_it4.559
r_mcbond_it2.894
r_angle_refined_deg1.823
r_nbtor_refined0.321
r_symmetry_vdw_refined0.304
r_nbd_refined0.224
r_symmetry_hbond_refined0.201
r_xyhbond_nbd_refined0.163
r_chiral_restr0.118
r_bond_refined_d0.019
r_gen_planes_refined0.007
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 Atoms4757
Nucleic Acid Atoms
Solvent Atoms135
Heterogen Atoms46

Software

Software
Software NamePurpose
CrystalCleardata collection
MOLREPphasing
REFMACrefinement
MOSFLMdata reduction
SCALAdata scaling