1XH9

Crystal Structures of Protein Kinase B Selective Inhibitors in Complex with Protein Kinase A and Mutants


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP6.4278LiCl, MesBisTris, methanol, MEGA-8, pH 6.4, VAPOR DIFFUSION, HANGING DROP, temperature 278K
Crystal Properties
Matthews coefficientSolvent content
2.2144.2

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 61.768α = 90
b = 78.787β = 90
c = 78.853γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMARRESEARCH2003-02-20MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONMPG/DESY, HAMBURG BEAMLINE BW61.05MPG/DESY, HAMBURGBW6

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
11.64355.9024651546515

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 REPLACEMENTTHROUGHOUT1.641644150236297.930.165820.164060.19859RANDOM14.971
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]
-0.31-0.060.37
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_1_deg5.689
r_scangle_it3.434
r_scbond_it2.147
r_mcangle_it1.441
r_angle_refined_deg1.345
r_angle_other_deg0.817
r_mcbond_it0.782
r_symmetry_vdw_refined0.386
r_symmetry_vdw_other0.304
r_nbd_other0.242
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_1_deg5.689
r_scangle_it3.434
r_scbond_it2.147
r_mcangle_it1.441
r_angle_refined_deg1.345
r_angle_other_deg0.817
r_mcbond_it0.782
r_symmetry_vdw_refined0.386
r_symmetry_vdw_other0.304
r_nbd_other0.242
r_nbd_refined0.212
r_xyhbond_nbd_refined0.147
r_symmetry_hbond_refined0.146
r_chiral_restr0.087
r_nbtor_other0.081
r_bond_refined_d0.012
r_gen_planes_refined0.007
r_gen_planes_other0.006
r_bond_other_d0.002
r_dihedral_angle_2_deg
r_dihedral_angle_3_deg
r_dihedral_angle_4_deg
r_nbtor_refined
r_xyhbond_nbd_other
r_metal_ion_refined
r_metal_ion_other
r_symmetry_hbond_other
r_mcbond_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms2920
Nucleic Acid Atoms
Solvent Atoms336
Heterogen Atoms58

Software

Software
Software NamePurpose
REFMACrefinement
MOSFLMdata reduction
CCP4data scaling
AMoREphasing