6PGX

Synthesis of novel tellurides bearing benzensulfonamide moiety as carbonic anhydrase inhibitors with antitumor activity


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, SITTING DROP281250 nL 7.5 mg/mL protein + 225 nL well solution (2.5-3.0 M ammonium sulfate, 100 mM Tris buffer, pH 8.0-8.5) + 25 nL microseeds
Crystal Properties
Matthews coefficientSolvent content
2.141.54

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 42.458α = 90
b = 41.38β = 104.41
c = 72.43γ = 90
Symmetry
Space GroupP 1 21 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 210r2018-02-14MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONAUSTRALIAN SYNCHROTRON BEAMLINE MX10.953700Australian SynchrotronMX1

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Merge I (Observed)Rpim 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
11.3641.497.60.0710.0280.99915.37.151332
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R Merge I (Observed)Rpim I (All)CC (Half)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
11.361.3892.40.4840.1990.8933.56.6

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 6ODZ1.3640.1348780253797.340.119440.117810.15237RANDOM13.65
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]
-0.22-0.140.070.19
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.598
r_dihedral_angle_4_deg23.532
r_dihedral_angle_3_deg11.764
r_dihedral_angle_1_deg6.895
r_long_range_B_refined3.236
r_long_range_B_other3.236
r_scangle_other2.467
r_scbond_it2.066
r_scbond_other2.066
r_angle_refined_deg1.85
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.598
r_dihedral_angle_4_deg23.532
r_dihedral_angle_3_deg11.764
r_dihedral_angle_1_deg6.895
r_long_range_B_refined3.236
r_long_range_B_other3.236
r_scangle_other2.467
r_scbond_it2.066
r_scbond_other2.066
r_angle_refined_deg1.85
r_rigid_bond_restr1.771
r_mcangle_other1.606
r_mcangle_it1.602
r_angle_other_deg1.535
r_mcbond_it1.174
r_mcbond_other1.17
r_chiral_restr0.093
r_bond_refined_d0.011
r_gen_planes_refined0.009
r_bond_other_d0.002
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_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms2064
Nucleic Acid Atoms
Solvent Atoms268
Heterogen Atoms76

Software

Software
Software NamePurpose
REFMACrefinement
XDSdata reduction
Aimlessdata scaling
PHASERphasing