5P9W

rat catechol O-methyltransferase in complex with 4'-fluoro-4,5-dihydroxy-N-{[(1R,2R)-2-{(2S,4R,5R)-4-hydroxy-5-[6-(methylamino)-9H-purin-9-yl]oxolan-2-yl}cyclopropyl]methyl}[1,1'-biphenyl]-3-carboxamide


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, SITTING DROP9295AMMONIUM SULPHATE, CHES, PH 9
Crystal Properties
Matthews coefficientSolvent content
2.2144.47

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 49.814α = 90
b = 54.366β = 90
c = 81.04γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMARMOSAIC 225 mm CCD2009-08-13MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSLS BEAMLINE X10SA1.000000SLSX10SA

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
11.4345.1599.30.10110.744.4441178-319.79
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)
11.431.4798.50.9491.39

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 REPLACEMENTTHROUGHOUTINHOUSE MODEL1.4345.1536362194192.50.1590.1580.191RANDOM11.27
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]
0.130.17-0.3
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg39.86
r_dihedral_angle_4_deg16.372
r_dihedral_angle_3_deg12.312
r_dihedral_angle_1_deg5.13
r_scangle_it4.104
r_scbond_it2.683
r_angle_refined_deg1.709
r_mcangle_it1.55
r_angle_other_deg1.085
r_mcbond_it0.943
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg39.86
r_dihedral_angle_4_deg16.372
r_dihedral_angle_3_deg12.312
r_dihedral_angle_1_deg5.13
r_scangle_it4.104
r_scbond_it2.683
r_angle_refined_deg1.709
r_mcangle_it1.55
r_angle_other_deg1.085
r_mcbond_it0.943
r_mcbond_other0.284
r_chiral_restr0.1
r_bond_refined_d0.018
r_gen_planes_refined0.009
r_bond_other_d0.001
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_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 Atoms1679
Nucleic Acid Atoms
Solvent Atoms246
Heterogen Atoms78

Software

Software
Software NamePurpose
REFMACrefinement
XSCALEdata scaling
PDB_EXTRACTdata extraction
XDSdata reduction
PHASERphasing