1XH8

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
2.3247

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 70.658α = 90
b = 73.111β = 90
c = 78.15γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMARRESEARCH2002-11-25MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONMPG/DESY, HAMBURG BEAMLINE BW61.00076MPG/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
11.622.534694346943

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 REPLACEMENTTHROUGHOUT1.622.5344536240492.590.201680.199860.2356RANDOM13.429
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]
-0.18-0.460.64
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_1_deg5.38
r_scangle_it3.681
r_scbond_it2.354
r_mcangle_it1.488
r_angle_refined_deg1.421
r_angle_other_deg0.823
r_mcbond_it0.82
r_symmetry_hbond_refined0.412
r_symmetry_vdw_other0.288
r_nbd_other0.245
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_1_deg5.38
r_scangle_it3.681
r_scbond_it2.354
r_mcangle_it1.488
r_angle_refined_deg1.421
r_angle_other_deg0.823
r_mcbond_it0.82
r_symmetry_hbond_refined0.412
r_symmetry_vdw_other0.288
r_nbd_other0.245
r_nbd_refined0.215
r_xyhbond_nbd_refined0.178
r_symmetry_vdw_refined0.144
r_chiral_restr0.092
r_nbtor_other0.085
r_bond_refined_d0.014
r_gen_planes_refined0.008
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 Atoms2961
Nucleic Acid Atoms
Solvent Atoms398
Heterogen Atoms42

Software

Software
Software NamePurpose
REFMACrefinement
MOSFLMdata reduction
CCP4data scaling
AMoREphasing