4AP7

Crystal structure of C-MET kinase domain in complex with 4-((6-(4- fluorophenyl)-(1,2,4)triazolo(4,3-b)(1,2,4)triazin-3-yl)methyl)phenol


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP4.6286CRYSTALS WERE OBTAINED AT 13 DEGRESS C IN 1-5 DAYS FROM HANGING DROPS CONTAINING 1.2 MICROLITERS OF PROTEIN: COMPOUND SOLUTION (1:5 MOLAR RATIO) AND 1.2 MICROLITERS OF PRECIPITATING SOLUTION (0.05 M CITRATE-PHOSPHATE, PH 4.6, 0-25 MM NACL, 21 % (W/V) PEG-3350). TO OBTAIN LARGER CRYSTALS, STREAK SEEDING WAS EMPLOYED USING THE CRYSTALS JUST MENTIONED AS DONORS, UNDER THE SAME CONDITIONS EXCEPT 275 MM NACL WAS USED AND THE DROPS WERE EQUILIBRATED OVERNIGHT BEFORE SEEDING WAS PERFORMED
Crystal Properties
Matthews coefficientSolvent content
2.3848.4

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 76.708α = 90
b = 93.387β = 90
c = 46.37γ = 90
Symmetry
Space GroupP 21 21 2

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray77CCDADSC QUANTUM 3152005-01-31MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONALS BEAMLINE 5.0.2ALS5.0.2

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
11.755095.90.08173.833132115.6
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)
11.751.8174.60.631.22.8

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodResolution (High)Resolution (Low)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-WorkR-FreeR-Free Selection DetailsMean Isotropic B
X-RAY DIFFRACTIONMOLECULAR REPLACEMENTTHROUGHOUT1.841.532862685790.50.1910.214RANDOM30.6
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]
-1.03-10.6911.73
RMS Deviations
KeyRefinement Restraint Deviation
c_dihedral_angle_d19.7
c_scangle_it3.17
c_scbond_it2.24
c_mcangle_it2.02
c_mcbond_it1.31
c_angle_deg0.8
c_improper_angle_d0.58
c_bond_d0.005
c_bond_d_na
c_bond_d_prot
RMS Deviations
KeyRefinement Restraint Deviation
c_dihedral_angle_d19.7
c_scangle_it3.17
c_scbond_it2.24
c_mcangle_it2.02
c_mcbond_it1.31
c_angle_deg0.8
c_improper_angle_d0.58
c_bond_d0.005
c_bond_d_na
c_bond_d_prot
c_angle_d
c_angle_d_na
c_angle_d_prot
c_angle_deg_na
c_angle_deg_prot
c_dihedral_angle_d_na
c_dihedral_angle_d_prot
c_improper_angle_d_na
c_improper_angle_d_prot
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms2309
Nucleic Acid Atoms
Solvent Atoms299
Heterogen Atoms24

Software

Software
Software NamePurpose
CNXrefinement
HKL-2000data reduction
SCALEPACKdata scaling
EPMRphasing