3PK2

Artificial Transfer Hydrogenases for the Enantioselective Reduction of Cyclic Imines


X-RAY DIFFRACTION

Starting Model(s)

Initial Refinement Model(s)
TypeSourceAccession CodeDetails
experimental modelPDB 2QCB 

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP42983.5 uL precipitation buffer (2.0 M ammonium sulfate, 0.1 M sodium acetate) mixed with 6.5 uL protein (26 mg/mL) and equilibrated against precipitation buffer, pH 4.0, VAPOR DIFFUSION, HANGING DROP, temperature 298K
Crystal Properties
Matthews coefficientSolvent content
2.3146.67

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 57.616α = 90
b = 57.616β = 90
c = 184.031γ = 90
Symmetry
Space GroupI 41 2 2

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDMARMOSAIC 225 mm CCD2009-09-17MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSLS BEAMLINE X06DA0.9793SLSX06DA

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
11.94691.20.1099.75.511601217.5
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)
1.9287.40.2014.541561

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodStarting modelResolution (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 REPLACEMENTTHROUGHOUT2qcb1.930116011101355990.90.185020.184010.20445RANDOM18.069
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]
-0.66-0.661.31
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg20.92
r_dihedral_angle_3_deg10.958
r_dihedral_angle_4_deg7.811
r_dihedral_angle_1_deg6.052
r_angle_refined_deg2.235
r_scangle_it1.978
r_angle_other_deg1.541
r_scbond_it1.269
r_mcangle_it0.864
r_mcbond_it0.471
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg20.92
r_dihedral_angle_3_deg10.958
r_dihedral_angle_4_deg7.811
r_dihedral_angle_1_deg6.052
r_angle_refined_deg2.235
r_scangle_it1.978
r_angle_other_deg1.541
r_scbond_it1.269
r_mcangle_it0.864
r_mcbond_it0.471
r_chiral_restr0.208
r_mcbond_other0.09
r_bond_refined_d0.011
r_gen_planes_refined0.006
r_bond_other_d
r_gen_planes_other
r_nbd_refined
r_nbd_other
r_nbtor_refined
r_nbtor_other
r_xyhbond_nbd_refined
r_xyhbond_nbd_other
r_metal_ion_refined
r_metal_ion_other
r_symmetry_vdw_refined
r_symmetry_vdw_other
r_symmetry_hbond_refined
r_symmetry_hbond_other
r_symmetry_metal_ion_refined
r_symmetry_metal_ion_other
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms912
Nucleic Acid Atoms
Solvent Atoms68
Heterogen Atoms43

Software

Software
Software NamePurpose
REFMACrefinement
MOSFLMdata reduction
SCALAdata scaling