2X6F

THE CRYSTAL STRUCTURE OF THE DROSOPHILA CLASS III PI3-KINASE VPS34 IN COMPLEX WITH 3-METHYLADENINE


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
17.5PROTEIN WAS CRYSTALLISED IN 0.88M AMMONIUM SULPHATE, 100MM DI-POTASSIUM HYDROGEN PHOSPHATE AND 100MM DI-SODIUM HYDROGEN PHOSPHATE (TITRATED TO PH 7.5 WITH ORTHOPHOSPHORIC ACID). PROTEIN WAS SOAKED WITH 1MM 3-MA IN MOTHER LIQUOR.
Crystal Properties
Matthews coefficientSolvent content
4.2670.92

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 112.07α = 90
b = 155.14β = 90
c = 244.53γ = 90
Symmetry
Space GroupI 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 315r2009-07-11MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONESRF BEAMLINE ID23-1ESRFID23-1

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
13.372.9298.20.14.993.6316651
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)
13.33.4899.70.691.043.66

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodStarting modelResolution (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 DIFFRACTIONMOLECULAR REPLACEMENTTHROUGHOUTPDB ENTRY 2X6H3.361.1330097156497.50.2450.2420.293RANDOM90.96
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]
2.942.09-5.03
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg38.727
r_dihedral_angle_1_deg25.474
r_dihedral_angle_3_deg22.413
r_dihedral_angle_4_deg19.064
r_scangle_it1.859
r_mcangle_it1.815
r_angle_refined_deg1.647
r_mcbond_it1.201
r_scbond_it1.042
r_symmetry_vdw_refined0.473
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg38.727
r_dihedral_angle_1_deg25.474
r_dihedral_angle_3_deg22.413
r_dihedral_angle_4_deg19.064
r_scangle_it1.859
r_mcangle_it1.815
r_angle_refined_deg1.647
r_mcbond_it1.201
r_scbond_it1.042
r_symmetry_vdw_refined0.473
r_symmetry_hbond_refined0.444
r_nbtor_refined0.326
r_nbd_refined0.3
r_xyhbond_nbd_refined0.249
r_chiral_restr0.1
r_bond_refined_d0.011
r_gen_planes_refined0.009
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_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 Atoms8875
Nucleic Acid Atoms
Solvent Atoms
Heterogen Atoms22

Software

Software
Software NamePurpose
REFMACrefinement
iMOSFLMdata reduction
SCALAdata scaling
PHASERphasing