4CFN

Structure-based design of C8-substituted O6-cyclohexylmethoxyguanine CDK1 and 2 inhibitors.


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
150 MM AMMONIUM ACETATE, 10% PEG-3350, 15 MM NACL, 100 MM HEPES, PH = 7.4, 10% DMSO
Crystal Properties
Matthews coefficientSolvent content
2.8757.16

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 73.981α = 90
b = 134.416β = 90
c = 147.865γ = 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 ID14-2ESRFID14-2

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
12.22.32920.0710.82.3368917
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)
12.22.3277.40.422.1

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodStarting modelResolution (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 REPLACEMENTTHROUGHOUTPDB ENTRY 1H1S2.299.565427346391.170.199320.197140.24087RANDOM36.479
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]
-0.11-1.821.93
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg42.02
r_dihedral_angle_3_deg17.517
r_dihedral_angle_4_deg17.412
r_dihedral_angle_1_deg6.321
r_angle_other_deg2.492
r_angle_refined_deg1.826
r_mcangle_it0.947
r_scbond_it0.741
r_mcbond_it0.611
r_mcbond_other0.611
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg42.02
r_dihedral_angle_3_deg17.517
r_dihedral_angle_4_deg17.412
r_dihedral_angle_1_deg6.321
r_angle_other_deg2.492
r_angle_refined_deg1.826
r_mcangle_it0.947
r_scbond_it0.741
r_mcbond_it0.611
r_mcbond_other0.611
r_chiral_restr0.161
r_bond_refined_d0.017
r_gen_planes_refined0.008
r_gen_planes_other0.008
r_bond_other_d0.002
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_it
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 Atoms8880
Nucleic Acid Atoms
Solvent Atoms555
Heterogen Atoms60

Software

Software
Software NamePurpose
REFMACrefinement
MOSFLMdata reduction
SCALAdata scaling
PHASERphasing