2X39

Structure of 4-Amino-N-(4-chlorobenzyl)-1-(7H-pyrrolo(2,3-d)pyrimidin- 4-yl)piperidine-4-carboxamide bound to PKB


X-RAY DIFFRACTION

Crystallization

Crystal Properties
Matthews coefficientSolvent content
2.2144.47

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 45.273α = 90
b = 60.518β = 90
c = 132.592γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC CCDMSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONESRF BEAMLINE ID23-1ESRFID23-1

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
11.9355.1970.096.13.227266
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)
11.932920.342

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 REPLACEMENTTHROUGHOUT1.9365.9425875134996.60.1690.1660.226RANDOM28.39
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]
-1.46-0.411.87
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg34.713
r_dihedral_angle_4_deg21.745
r_dihedral_angle_3_deg13.648
r_scangle_it8.565
r_dihedral_angle_1_deg5.964
r_scbond_it5.782
r_mcangle_it5.636
r_mcbond_it3.35
r_angle_refined_deg1.479
r_angle_other_deg0.892
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg34.713
r_dihedral_angle_4_deg21.745
r_dihedral_angle_3_deg13.648
r_scangle_it8.565
r_dihedral_angle_1_deg5.964
r_scbond_it5.782
r_mcangle_it5.636
r_mcbond_it3.35
r_angle_refined_deg1.479
r_angle_other_deg0.892
r_chiral_restr0.092
r_bond_refined_d0.015
r_gen_planes_refined0.007
r_gen_planes_other0.002
r_bond_other_d0.001
r_mcbond_other0.001
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_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 Atoms2670
Nucleic Acid Atoms
Solvent Atoms246
Heterogen Atoms27

Software

Software
Software NamePurpose
REFMACrefinement
MOSFLMdata reduction
SCALAdata scaling