3G04

Crystal structure of the TSH receptor in complex with a thyroid-stimulating autoantibody


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP62928% PEG 8000, 0.1M MES, 0.25M ZINC ACETATE, pH 6.00, VAPOR DIFFUSION, HANGING DROP, temperature 292K
Crystal Properties
Matthews coefficientSolvent content
2.6653.82

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 43.888α = 90
b = 175.784β = 90
c = 205.806γ = 90
Symmetry
Space GroupI 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 42006-11-06MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSRS BEAMLINE PX14.20.98SRSPX14.2

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Merge I (Observed)R Sym 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
12.553096.10.0710.07110.54.626775257312.547.7
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R Merge I (Observed)R-Sym I (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
12.552.6199.20.3610.3614.4

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 REPLACEMENTTHROUGHOUTPDB ENTRY 1XWD2.5526.72244261301960.1840.1810.245RANDOM36
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]
0.16-0.190.03
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg39.599
r_dihedral_angle_4_deg18.934
r_dihedral_angle_3_deg16.207
r_dihedral_angle_1_deg6.528
r_scangle_it3.392
r_mcangle_it2.673
r_scbond_it2.261
r_mcbond_it1.775
r_angle_refined_deg1.236
r_nbtor_refined0.306
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg39.599
r_dihedral_angle_4_deg18.934
r_dihedral_angle_3_deg16.207
r_dihedral_angle_1_deg6.528
r_scangle_it3.392
r_mcangle_it2.673
r_scbond_it2.261
r_mcbond_it1.775
r_angle_refined_deg1.236
r_nbtor_refined0.306
r_symmetry_vdw_refined0.25
r_nbd_refined0.201
r_metal_ion_refined0.177
r_symmetry_hbond_refined0.164
r_xyhbond_nbd_refined0.146
r_chiral_restr0.082
r_symmetry_metal_ion_refined0.046
r_bond_refined_d0.009
r_gen_planes_refined0.003
r_bond_other_d
r_angle_other_deg
r_gen_planes_other
r_nbd_other
r_nbtor_other
r_xyhbond_nbd_other
r_metal_ion_other
r_symmetry_vdw_other
r_symmetry_hbond_other
r_symmetry_metal_ion_other
r_mcbond_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms5036
Nucleic Acid Atoms
Solvent Atoms289
Heterogen Atoms89

Software

Software
Software NamePurpose
PXGENdata collection
AMoREphasing
REFMACrefinement
DENZOdata reduction
SCALEPACKdata scaling