3CDA

Thermodynamic and structure guided design of statin hmg-coa reductase inhibitors


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP8293protein 15-20 mg/ml, Ligand (saturated),PEG 4000, MgCl2 0.2M, Tris-HCL pH8 0.1M, 7-10 days, pH 8.0, VAPOR DIFFUSION, HANGING DROP, temperature 293K
Crystal Properties
Matthews coefficientSolvent content
2.244.03

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 72.611α = 90
b = 172.249β = 118.04
c = 75.62γ = 90
Symmetry
Space GroupP 1 21 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMAR CCD 165 mm2003-06-19MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONAPS BEAMLINE 17-BM1.0000APS17-BM

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
12.075090.70.0661390237
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)
2.082.1578.20.1997736

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 DIFFRACTIONTHROUGHOUT2.075090191206690.460.2140.2130.257RANDOM34.538
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]
2.18-2.89-3.21-1.69
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_1_deg5.669
r_scangle_it1.756
r_angle_refined_deg1.196
r_scbond_it1.023
r_mcangle_it0.752
r_angle_other_deg0.747
r_mcbond_it0.399
r_nbd_other0.216
r_symmetry_vdw_other0.197
r_nbd_refined0.184
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_1_deg5.669
r_scangle_it1.756
r_angle_refined_deg1.196
r_scbond_it1.023
r_mcangle_it0.752
r_angle_other_deg0.747
r_mcbond_it0.399
r_nbd_other0.216
r_symmetry_vdw_other0.197
r_nbd_refined0.184
r_symmetry_hbond_refined0.165
r_symmetry_vdw_refined0.161
r_xyhbond_nbd_refined0.158
r_nbtor_other0.08
r_chiral_restr0.06
r_bond_refined_d0.008
r_gen_planes_refined0.003
r_bond_other_d0.002
r_gen_planes_other0.002
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms12298
Nucleic Acid Atoms
Solvent Atoms493
Heterogen Atoms180

Software

Software
Software NamePurpose
DENZOdata reduction
SCALEPACKdata scaling
REFMACrefinement
PDB_EXTRACTdata extraction