4NMH

11-beta-HSD1 in complex with a 3,3-Di-methyl-azetidin-2-one


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP5.52931.9 M ammonium sulphate, 0.1 M citrate at pH 5.5, VAPOR DIFFUSION, HANGING DROP, temperature 293K
Crystal Properties
Matthews coefficientSolvent content
2.4750.27

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 96.132α = 90
b = 70.842β = 91.67
c = 95.653γ = 90
Symmetry
Space GroupP 1 21 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 210toroidal mirror2006-08-03MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONESRF BEAMLINE ID291.037ESRFID29

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
12.996.2387.80.1543.92.8252452524540.3
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)
12.93.0680.80.4461.42.63360

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodResolution (High)Resolution (Low)Number Reflections (All)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-Factor (All)R-Factor (Observed)R-WorkR-FreeR-Free Selection DetailsMean Isotropic B
X-RAY DIFFRACTIONMOLECULAR REPLACEMENTTHROUGHOUT2.996.232522825228129487.60.201320.201320.198670.25139RANDOM21.177
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]
0.64-2.69-2.531.73
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg30.288
r_dihedral_angle_4_deg14.009
r_dihedral_angle_3_deg13.65
r_dihedral_angle_1_deg4.858
r_scangle_it2.576
r_scbond_it1.746
r_angle_other_deg1.592
r_mcangle_it1.097
r_mcbond_it0.956
r_angle_refined_deg0.902
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg30.288
r_dihedral_angle_4_deg14.009
r_dihedral_angle_3_deg13.65
r_dihedral_angle_1_deg4.858
r_scangle_it2.576
r_scbond_it1.746
r_angle_other_deg1.592
r_mcangle_it1.097
r_mcbond_it0.956
r_angle_refined_deg0.902
r_nbd_refined0.181
r_nbd_other0.173
r_nbtor_refined0.172
r_symmetry_vdw_refined0.139
r_symmetry_vdw_other0.13
r_xyhbond_nbd_refined0.118
r_symmetry_hbond_refined0.1
r_nbtor_other0.076
r_chiral_restr0.048
r_mcbond_other0.027
r_bond_refined_d0.006
r_gen_planes_refined0.003
r_bond_other_d0.001
r_gen_planes_other0.001
r_xyhbond_nbd_other
r_metal_ion_refined
r_metal_ion_other
r_symmetry_hbond_other
r_symmetry_metal_ion_refined
r_symmetry_metal_ion_other
r_mcangle_other
r_scbond_other
r_scangle_other
r_long_range_B_refined
r_long_range_B_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms8142
Nucleic Acid Atoms
Solvent Atoms33
Heterogen Atoms322

Software

Software
Software NamePurpose
ADSCdata collection
MOLREPphasing
REFMACrefinement
XDSdata reduction
XSCALEdata scaling