1C2K

RECRUITING ZINC TO MEDIATE POTENT, SPECIFIC INHIBITION OF SERINE PROTEASES


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
13.85BATCH, 1.51 M MGSO4 . 7 H2O, 0.59 MM TRYPSIN, 1.0 MM ZN(II) 5.0 % DMSO: CRYSTALLIZATION SOLUTION WAS SATURATED IN KETO-BABIM. CRYSTAL WAS TRANSFERRED TO SYNTHETIC MOTHER LIQUOR CONTAINING 2.11 M ZN(II), PH 3.85 AND SOAKED FOR SEVERAL DAYS WITH SEVERAL REPLACEMENTS OF SOAKING SOLUTIONS. THE SOLUTION WAS SATURATED IN KETO-BABIM AND CONTAINED 2.0 % DMSO TO INCREASE INHIBITOR SOLUBILITY. UNDER THIS CONDITION KETO-BABIM UNDERGOES DECOMPOSITION TO 5- AMIDINO-BENZIMIDAZOLE.
Crystal Properties
Matthews coefficientSolvent content
2.0318

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 54.91α = 90
b = 54.91β = 90
c = 108.93γ = 120
Symmetry
Space GroupP 31 2 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray298IMAGE PLATERIGAKU RAXIS IV++MSC MIRRORS1997-01-13MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1ROTATING ANODE

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
11.4543.58680.0826.42.9173801.2
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)
1.651.7232.80.271.6

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodResolution (High)Resolution (Low)Cut-off Sigma (F)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-Factor (Observed)R-WorkR-FreeMean Isotropic B
X-RAY DIFFRACTIONDIFFERENCE FOURIER PLUS REFINEMENTX-PLOR1.657.52158361599680.2020.2020.243
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]
RMS Deviations
KeyRefinement Restraint Deviation
x_dihedral_angle_d26.1
x_angle_deg3.9
x_improper_angle_d0.5
x_bond_d0.018
x_bond_d_na
x_bond_d_prot
x_angle_d
x_angle_d_na
x_angle_d_prot
x_angle_deg_na
RMS Deviations
KeyRefinement Restraint Deviation
x_dihedral_angle_d26.1
x_angle_deg3.9
x_improper_angle_d0.5
x_bond_d0.018
x_bond_d_na
x_bond_d_prot
x_angle_d
x_angle_d_na
x_angle_d_prot
x_angle_deg_na
x_angle_deg_prot
x_dihedral_angle_d_na
x_dihedral_angle_d_prot
x_improper_angle_d_na
x_improper_angle_d_prot
x_mcbond_it
x_mcangle_it
x_scbond_it
x_scangle_it
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms3331
Nucleic Acid Atoms
Solvent Atoms564
Heterogen Atoms25

Software

Software
Software NamePurpose
bioteXdata collection
bioteXdata reduction
X-PLORmodel building
Quantamodel building
Insight IImodel building
X-PLORrefinement
bioteXdata scaling
X-PLORphasing