3IW4

Crystal structure of PKC alpha in complex with NVP-AEB071


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP5.1278protein solution: 12mg/mL in 0.2M NaCl, 0.05M imidazole, pH8.0, 2mM TCEP, 1mM NAF, 2% glycerol, reservoir solution: 1mL 22% polyethyleneglycol 3350, 0.2M di-ammonium-hydrogen citrate, pH5.1, VAPOR DIFFUSION, HANGING DROP, temperature 278K
Crystal Properties
Matthews coefficientSolvent content
2.2244.72

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 43.868α = 90
b = 100.669β = 90
c = 251.335γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMARMOSAIC 225 mm CCD2006-06-01MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSLS BEAMLINE X10SA0.97880SLSX10SA

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
12.810099.50.1389.214.52833128331-345.933
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)
12.82.9298.50.6642.3

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 DIFFRACTIONFOURIER SYNTHESISTHROUGHOUT2.864.4226913141799.480.196250.192090.27703RANDOM39.781
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]
-1.331.46-0.13
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg37.039
r_dihedral_angle_4_deg21.062
r_dihedral_angle_3_deg19.114
r_dihedral_angle_1_deg6.517
r_scangle_it5.383
r_scbond_it3.531
r_mcangle_it2.233
r_angle_refined_deg1.424
r_mcbond_it1.136
r_chiral_restr0.088
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg37.039
r_dihedral_angle_4_deg21.062
r_dihedral_angle_3_deg19.114
r_dihedral_angle_1_deg6.517
r_scangle_it5.383
r_scbond_it3.531
r_mcangle_it2.233
r_angle_refined_deg1.424
r_mcbond_it1.136
r_chiral_restr0.088
r_bond_refined_d0.011
r_gen_planes_refined0.006
r_bond_other_d
r_angle_other_deg
r_gen_planes_other
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_mcbond_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms8051
Nucleic Acid Atoms
Solvent Atoms46
Heterogen Atoms99

Software

Software
Software NamePurpose
XSCALEdata scaling
REFMACrefinement
PDB_EXTRACTdata extraction
MAR345data collection
XDSdata reduction
REFMACphasing