3SN7

Highly Potent, Selective, and Orally Active Phosphodiestarase 10A Inhibitors


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP7.129112-18% PEG 3350, 100 mM MES pH 7.1, 3-6% Methanol, VAPOR DIFFUSION, HANGING DROP, temperature 291K
Crystal Properties
Matthews coefficientSolvent content
2.0640.23

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 50.641α = 90
b = 81.465β = 90
c = 158.044γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMARMOSAIC 300 mm CCD2008-08-04MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONAPS BEAMLINE 22-ID1.0APS22-ID

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (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
11.825079.3596784729111
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
11.821.8923.5

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodResolution (High)Resolution (Low)Cut-off Sigma (F)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 REPLACEMENTTHROUGHOUT1.8244.2415957144841241679.330.2480.2480.2470.276RANDOM32.175
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]
0.11-0.130.01
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg35.595
r_dihedral_angle_4_deg15.127
r_dihedral_angle_3_deg13.769
r_dihedral_angle_1_deg4.615
r_angle_refined_deg0.984
r_scangle_it0.976
r_mcangle_it0.685
r_scbond_it0.623
r_mcbond_it0.389
r_nbtor_refined0.292
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg35.595
r_dihedral_angle_4_deg15.127
r_dihedral_angle_3_deg13.769
r_dihedral_angle_1_deg4.615
r_angle_refined_deg0.984
r_scangle_it0.976
r_mcangle_it0.685
r_scbond_it0.623
r_mcbond_it0.389
r_nbtor_refined0.292
r_nbd_refined0.177
r_symmetry_vdw_refined0.177
r_symmetry_hbond_refined0.119
r_xyhbond_nbd_refined0.111
r_metal_ion_refined0.102
r_chiral_restr0.069
r_bond_refined_d0.007
r_gen_planes_refined0.003
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_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 Atoms5120
Nucleic Acid Atoms
Solvent Atoms256
Heterogen Atoms56

Software

Software
Software NamePurpose
MAR345data collection
SHARPphasing
REFMACrefinement
HKL-2000data reduction
HKL-2000data scaling