3QPV

PFKFB3 trapped in a phospho-enzyme intermediate state


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, SITTING DROP7.5300100 mM Tris-HCl,20-25% ethylene glycol, 200-400mM Tartaric Acid, 5% glycerol, and 12% polyethylene glycol 4000, pH 7.5, VAPOR DIFFUSION, SITTING DROP, temperature 300K
Crystal Properties
Matthews coefficientSolvent content
3.2762.42

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 102.146α = 90
b = 102.146β = 90
c = 259.439γ = 120
Symmetry
Space GroupP 65 2 2

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100IMAGE PLATEMAR scanner 345 mm plate2007-07-26MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONCAMD BEAMLINE GCPCC1.3808CAMDGCPCC

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
12.453099.6303813038111
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
12.452.5498.7

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 (Observed)R-WorkR-FreeR-Free Selection DetailsMean Isotropic B
X-RAY DIFFRACTIONMOLECULAR REPLACEMENTTHROUGHOUT2.5303038124542274195.430.199160.19370.2475RANDOM42.457
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]
0.440.220.44-0.66
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg37.867
r_dihedral_angle_4_deg20.446
r_dihedral_angle_3_deg18.834
r_dihedral_angle_1_deg6.816
r_scangle_it5.148
r_scbond_it3.357
r_mcangle_it2.201
r_angle_refined_deg2.179
r_mcbond_it1.346
r_nbtor_refined0.322
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg37.867
r_dihedral_angle_4_deg20.446
r_dihedral_angle_3_deg18.834
r_dihedral_angle_1_deg6.816
r_scangle_it5.148
r_scbond_it3.357
r_mcangle_it2.201
r_angle_refined_deg2.179
r_mcbond_it1.346
r_nbtor_refined0.322
r_nbd_refined0.263
r_symmetry_vdw_refined0.217
r_xyhbond_nbd_refined0.185
r_symmetry_hbond_refined0.177
r_chiral_restr0.143
r_bond_refined_d0.024
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_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms3597
Nucleic Acid Atoms
Solvent Atoms175
Heterogen Atoms67

Software

Software
Software NamePurpose
HKL-2000data collection
REFMACrefinement
HKL-2000data reduction
HKL-2000data scaling
REFMACphasing