3Q5G

Sulphur SAD structure solution of proteinase K grown in SO4 solution


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP6.52931 muL of 40 mg/ml protein mixed with 1 muL of the mother liquor. Mother liquor : 400 mM Ammonium SO4, 25 % glycerol, 100 mM Na cacodylate pH 6.5, VAPOR DIFFUSION, HANGING DROP, temperature 293K
Crystal Properties
Matthews coefficientSolvent content
2.0339.46

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 67.864α = 90
b = 67.864β = 90
c = 102.193γ = 90
Symmetry
Space GroupP 43 21 2

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 270Si(111) channel cut mono. Rh coated toroidal focusing mirror.2010-11-20MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONNSLS BEAMLINE X6A1.7712NSLSX6A

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
11.77301000.05390.925.424015240152211.7
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)
11.771.81000.15216.611.51175

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 DIFFRACTIONSADTHROUGHOUT1.77302273012261000.125960.123830.16658RANDOM10.457
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]
-0.08-0.080.17
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg38.018
r_dihedral_angle_4_deg15.933
r_dihedral_angle_3_deg11.698
r_dihedral_angle_1_deg5.892
r_scangle_it3.694
r_scbond_it2.281
r_angle_refined_deg1.372
r_mcangle_it1.217
r_mcbond_it0.713
r_chiral_restr0.109
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg38.018
r_dihedral_angle_4_deg15.933
r_dihedral_angle_3_deg11.698
r_dihedral_angle_1_deg5.892
r_scangle_it3.694
r_scbond_it2.281
r_angle_refined_deg1.372
r_mcangle_it1.217
r_mcbond_it0.713
r_chiral_restr0.109
r_bond_refined_d0.016
r_gen_planes_refined0.008
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms2031
Nucleic Acid Atoms
Solvent Atoms397
Heterogen Atoms12

Software

Software
Software NamePurpose
DCS_X6Adata collection
SHELXSphasing
REFMACrefinement
HKL-2000data reduction
HKL-2000data scaling