6H44

Flavin-dependent Tryptophan 6-halogenase Thal in complex with tryptophan


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
2VAPOR DIFFUSION, SITTING DROP92930.1 M bicine pH 9.0, 1.6 M K2HPO4/NaH2PO4 protein concentration: ~15 mg/mL protein buffer:10 mM Tris pH 7.4, 50 mM NaCl and 1 mM TCEP drop ratio: 1:1 (P:R)

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 136.7α = 90
b = 136.7β = 90
c = 144.9γ = 120
Symmetry
Space GroupP 64

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100PIXELDECTRIS PILATUS 6M-F2017-05-30MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONPETRA III, EMBL c/o DESY BEAMLINE P13 (MX1)0.9763PETRA III, EMBL c/o DESYP13 (MX1)

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)Rrim I (All)CC (Half)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
12.55501000.1720.99915.8920.595005652.5
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)Rrim I (All)CC (Half)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
12.552.621001.7760.6662.0720.74

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 REPLACEMENTTHROUGHOUTThal2.5549.7747558246299.930.181180.178920.22506RANDOM56.068
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]
0.450.220.45-1.46
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg31.638
r_dihedral_angle_4_deg21.376
r_dihedral_angle_3_deg15.009
r_long_range_B_refined8.907
r_long_range_B_other8.906
r_scangle_other7.06
r_dihedral_angle_1_deg6.791
r_mcangle_it6.356
r_mcangle_other6.355
r_scbond_it4.81
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg31.638
r_dihedral_angle_4_deg21.376
r_dihedral_angle_3_deg15.009
r_long_range_B_refined8.907
r_long_range_B_other8.906
r_scangle_other7.06
r_dihedral_angle_1_deg6.791
r_mcangle_it6.356
r_mcangle_other6.355
r_scbond_it4.81
r_scbond_other4.81
r_mcbond_it4.359
r_mcbond_other4.359
r_angle_refined_deg1.265
r_angle_other_deg0.875
r_chiral_restr0.061
r_bond_refined_d0.008
r_gen_planes_refined0.006
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_scangle_it
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms8432
Nucleic Acid Atoms
Solvent Atoms197
Heterogen Atoms150

Software

Software
Software NamePurpose
REFMACrefinement
XDSdata reduction
XSCALEdata scaling
PHASERphasing