3SUE

Crystal structure of NS3/4A protease variant R155K in complex with MK-5172


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1hanging drop, vapor diffusion6.229520-25% PEG 3350, 0.1M MES (pH 6.5), 4% ammonium sulfate, hanging drop, vapor diffusion, temperature 295K
Crystal Properties
Matthews coefficientSolvent content
2.346.5

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 56.335α = 90
b = 103.324β = 112.58
c = 73.498γ = 90
Symmetry
Space GroupP 1 21 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray1002011-03-16SINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1ROTATING ANODERIGAKU1.54

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
12.25091.60.0859.52.236194
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)
12.22.2894.10.362.2

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 REPLACEMENTTHROUGHOUT2.232.2434332181491.170.188320.186050.22924RANDOM33.039
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]
3.9-1.798.49-12.39
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg33.033
r_dihedral_angle_3_deg15.789
r_dihedral_angle_4_deg13.382
r_dihedral_angle_1_deg6.466
r_angle_other_deg1.306
r_angle_refined_deg1.289
r_scangle_it1.283
r_scbond_it0.81
r_mcangle_it0.419
r_mcbond_it0.23
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg33.033
r_dihedral_angle_3_deg15.789
r_dihedral_angle_4_deg13.382
r_dihedral_angle_1_deg6.466
r_angle_other_deg1.306
r_angle_refined_deg1.289
r_scangle_it1.283
r_scbond_it0.81
r_mcangle_it0.419
r_mcbond_it0.23
r_chiral_restr0.069
r_mcbond_other0.051
r_bond_refined_d0.009
r_bond_other_d0.008
r_gen_planes_refined0.006
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_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms5407
Nucleic Acid Atoms
Solvent Atoms151
Heterogen Atoms220

Software

Software
Software NamePurpose
DENZOdata reduction
SCALEPACKdata scaling
REFMACrefinement
PDB_EXTRACTdata extraction