4NKS

Crystal structure of human fibroblast growth factor receptor 1 kinase domain in complex with pyrazolaminopyrimidine 3


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP6.75277.1516-20% PEG 8000, 100mM PCTP, 100-300mM ammonium sulfate, 25% ethylene glycol, pH 6.75, VAPOR DIFFUSION, HANGING DROP, temperature 277.15K
Crystal Properties
Matthews coefficientSolvent content
2.6653.73

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 208.058α = 90
b = 56.918β = 107.73
c = 66.242γ = 90
Symmetry
Space GroupC 1 2 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 315rMSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONESRF BEAMLINE ID14-4ESRFID14-4

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
12.599.0197.40.0819.43.48502623909
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)
12.52.6498.50.4423.83.5

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 REPLACEMENTTHROUGHOUT2.599.0123909128697.380.222510.219580.27762RANDOM47.421
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]
-4-2.585.95-0.93
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.407
r_dihedral_angle_3_deg15.655
r_dihedral_angle_4_deg13.326
r_dihedral_angle_1_deg5.965
r_long_range_B_other4.595
r_long_range_B_refined4.594
r_scangle_other3.93
r_mcangle_it3.327
r_mcangle_other3.326
r_scbond_it2.944
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.407
r_dihedral_angle_3_deg15.655
r_dihedral_angle_4_deg13.326
r_dihedral_angle_1_deg5.965
r_long_range_B_other4.595
r_long_range_B_refined4.594
r_scangle_other3.93
r_mcangle_it3.327
r_mcangle_other3.326
r_scbond_it2.944
r_scbond_other2.944
r_mcbond_it2.575
r_mcbond_other2.575
r_angle_refined_deg1.46
r_angle_other_deg0.814
r_chiral_restr0.077
r_bond_refined_d0.013
r_gen_planes_refined0.006
r_bond_other_d0.005
r_gen_planes_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_scangle_it
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms4113
Nucleic Acid Atoms
Solvent Atoms22
Heterogen Atoms56

Software

Software
Software NamePurpose
AMoREphasing
REFMACrefinement
MOSFLMdata reduction
SCALAdata scaling