4RA5

Human Protein Kinase C THETA IN COMPLEX WITH LIGAND COMPOUND 11a (6-[(1,3-Dimethyl-azetidin-3-yl)-methyl-amino]-4(R)-methyl-7-phenyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one)


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP4.25PEG 3350, MgCl2, sodium acetate and sodium malonate, pH 4.25, VAPOR DIFFUSION, HANGING DROP
Crystal Properties
Matthews coefficientSolvent content
2.8356.55

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 74.822α = 90
b = 77.026β = 90
c = 147.547γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100PIXELDECTRIS PILATUS 6M2012-10-19MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSLS BEAMLINE X06SA1.00SLSX06SA

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
12.6173.7799.10.0473.726584
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)
12.612.8699.30.4443.8

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 DIFFRACTIONTHROUGHOUT2.6173.772543691299.110.229820.228170.27681RANDOM71.678
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]
8.66-4.38-4.28
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg33.011
r_dihedral_angle_4_deg15.432
r_dihedral_angle_3_deg13.406
r_dihedral_angle_1_deg6.004
r_scangle_it3.375
r_scbond_it2.228
r_mcangle_it1.476
r_angle_refined_deg1.123
r_angle_other_deg0.914
r_mcbond_it0.822
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg33.011
r_dihedral_angle_4_deg15.432
r_dihedral_angle_3_deg13.406
r_dihedral_angle_1_deg6.004
r_scangle_it3.375
r_scbond_it2.228
r_mcangle_it1.476
r_angle_refined_deg1.123
r_angle_other_deg0.914
r_mcbond_it0.822
r_nbtor_refined0.161
r_nbd_refined0.158
r_mcbond_other0.157
r_nbd_other0.129
r_xyhbond_nbd_refined0.119
r_symmetry_vdw_other0.094
r_symmetry_hbond_refined0.082
r_nbtor_other0.073
r_chiral_restr0.068
r_symmetry_vdw_refined0.041
r_metal_ion_refined0.04
r_bond_refined_d0.009
r_gen_planes_refined0.003
r_bond_other_d0.002
r_gen_planes_other0.001
r_xyhbond_nbd_other
r_metal_ion_other
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 Atoms5375
Nucleic Acid Atoms
Solvent Atoms24
Heterogen Atoms69

Software

Software
Software NamePurpose
REFMACrefinement
XDSdata reduction
XSCALEdata scaling