2CMY

Crystal complex between bovine trypsin and Veronica hederifolia trypsin inhibitor


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
18CRYSTALS OF TRYPSIN WERE GROWN IN 2.5M AMMONIUM SULPHATE, 6MM CALCIUM CHLORIDE, 0.1M TRIS PH 8.15, 60MM BENZAMIDINE. THEY WERE BACKSOAKED IN 0.1M NA PHOSPHATE PH 5.8, 2.5M AMMONIUM SULPHATE TO REMOVE BENZAMIDINE. CRYSTALS WERE MOVED TO 2.5M AMMONIUM SULPHATE, 1MM CALCIUM CHLORDIE, 0.1M TRIS PH 8 AND PEPTIDE INHIBITOR ADDED AT 10MM AND INCUBATED FOR 16 HOURS.
Crystal Properties
Matthews coefficientSolvent content
2.5851.96

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 60.657α = 90
b = 63.928β = 90
c = 71.698γ = 90
Symmetry
Space GroupP 21 21 21

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 4MIRROR2003-10-05MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSRS BEAMLINE PX14.1SRSPX14.1

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
12.2547.7397.50.1211.94.2133421.4
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)
12.252.3384.90.591.43.6

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 1SFI2.2547.731268166196.90.1960.1940.253RANDOM73.66
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]
3.66-2.78-0.88
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg41.14
r_dihedral_angle_4_deg21.147
r_dihedral_angle_3_deg15.568
r_dihedral_angle_1_deg7.853
r_scangle_it3.316
r_scbond_it2.481
r_angle_refined_deg1.887
r_mcangle_it1.555
r_mcbond_it0.93
r_nbtor_refined0.301
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg41.14
r_dihedral_angle_4_deg21.147
r_dihedral_angle_3_deg15.568
r_dihedral_angle_1_deg7.853
r_scangle_it3.316
r_scbond_it2.481
r_angle_refined_deg1.887
r_mcangle_it1.555
r_mcbond_it0.93
r_nbtor_refined0.301
r_symmetry_hbond_refined0.276
r_nbd_refined0.239
r_xyhbond_nbd_refined0.18
r_symmetry_vdw_refined0.179
r_chiral_restr0.13
r_bond_refined_d0.022
r_gen_planes_refined0.007
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 Atoms1798
Nucleic Acid Atoms
Solvent Atoms110
Heterogen Atoms17

Software

Software
Software NamePurpose
REFMACrefinement
HKL-2000data reduction
SCALEPACKdata scaling
AMoREphasing