3G70

Design and Preparation of Potent, Non-Peptidic, Bioavailable Renin Inhibitors


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, SITTING DROP4.529325-30% PEG 4000, 0.6M NaCl, 0.1M Citrate(pH 4-5), VAPOR DIFFUSION, SITTING DROP, temperature 293K
Crystal Properties
Matthews coefficientSolvent content
2.3347.12

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 65.73α = 90
b = 89.46β = 90
c = 118.37γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100IMAGE PLATEMAR scanner 345 mm plate2004-11-15MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSLS BEAMLINE X06SA1.0SLSX06SA

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
1270850.0752.640473

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 REPLACEMENTTHROUGHOUT236.984047338393204284.410.220.199470.196060.26291RANDOM36.102
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]
0.261.44-1.7
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.464
r_dihedral_angle_4_deg19.542
r_dihedral_angle_3_deg16.968
r_dihedral_angle_1_deg6.911
r_scangle_it3.273
r_mcangle_it2.809
r_scbond_it2.209
r_mcbond_it1.923
r_angle_refined_deg1.488
r_nbtor_refined0.308
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg36.464
r_dihedral_angle_4_deg19.542
r_dihedral_angle_3_deg16.968
r_dihedral_angle_1_deg6.911
r_scangle_it3.273
r_mcangle_it2.809
r_scbond_it2.209
r_mcbond_it1.923
r_angle_refined_deg1.488
r_nbtor_refined0.308
r_symmetry_hbond_refined0.284
r_symmetry_vdw_refined0.216
r_nbd_refined0.209
r_xyhbond_nbd_refined0.165
r_chiral_restr0.096
r_bond_refined_d0.013
r_gen_planes_refined0.005
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_refined
r_metal_ion_other
r_symmetry_vdw_other
r_symmetry_hbond_other
r_symmetry_metal_ion_refined
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 Atoms5175
Nucleic Acid Atoms
Solvent Atoms374
Heterogen Atoms122

Software

Software
Software NamePurpose
MAR345dtbdata collection
MOLREPphasing
REFMACrefinement
MOSFLMdata reduction
SCALAdata scaling