5WEX

Discovery of new selenoureido analogs of 4-(4-fluorophenylureido) benzenesulfonamides as carbonic anhydrase inhibitors


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, SITTING DROP8.3281concentrated CA II at about 10 mg/mL was set up in SD-2 plates with the following ratio of protein plus reservoir plus seeds: 250nL plus 225 nL plus 25 nL. The plate was incubated at 8C and the reservoir condition consisted of 2.9 M ammonium sulfate with 0.1 M Tris buffer at pH 8. 3
Crystal Properties
Matthews coefficientSolvent content
2.1141.67

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 42.472α = 90
b = 41.502β = 104.39
c = 72.35γ = 90
Symmetry
Space GroupP 1 21 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100PIXELDECTRIS EIGER X 16M2017-03-15MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONAUSTRALIAN SYNCHROTRON BEAMLINE MX20.95372Australian SynchrotronMX2

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Merge I (Observed)R Sym 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
11.2641.196.90.0820.0890.0340.99910.66.863929
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R Merge I (Observed)R-Sym I (Observed)Rpim I (All)CC (Half)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
11.261.2893.41.1751.2860.5110.60926

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 DIFFRACTIONTHROUGHOUT1.2641.160631310896.390.11930.117850.14655RANDOM16.971
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]
-0.030.02-0.340.31
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.499
r_sphericity_free24.468
r_dihedral_angle_4_deg22.224
r_dihedral_angle_3_deg12.608
r_sphericity_bonded10.981
r_dihedral_angle_1_deg6.292
r_long_range_B_refined3.597
r_long_range_B_other3.597
r_scangle_other3.414
r_scbond_other2.996
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.499
r_sphericity_free24.468
r_dihedral_angle_4_deg22.224
r_dihedral_angle_3_deg12.608
r_sphericity_bonded10.981
r_dihedral_angle_1_deg6.292
r_long_range_B_refined3.597
r_long_range_B_other3.597
r_scangle_other3.414
r_scbond_other2.996
r_scbond_it2.989
r_rigid_bond_restr2.788
r_mcangle_other2.375
r_mcangle_it2.364
r_mcbond_it1.795
r_mcbond_other1.792
r_angle_refined_deg1.766
r_angle_other_deg1.03
r_chiral_restr0.131
r_bond_refined_d0.015
r_gen_planes_refined0.01
r_bond_other_d0.002
r_gen_planes_other0.002
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
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms2049
Nucleic Acid Atoms
Solvent Atoms237
Heterogen Atoms32

Software

Software
Software NamePurpose
REFMACrefinement
DIALSdata reduction
Aimlessdata scaling
PHASERphasing