3BOW

Structure of M-calpain in complex with Calpastatin


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
16.5298pH 6.5, microbatch under paraffin oil, temperature 298K
Crystal Properties
Matthews coefficientSolvent content
2.1242.05

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 67.477α = 90
b = 66.985β = 100.76
c = 108.656γ = 90
Symmetry
Space GroupP 1 21 1

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 210MIRRORS2007-04-24SINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONNSLS BEAMLINE X6ANSLSX6A

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Merge I (Observed)R Sym 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
12.466.96596.70.0840.0847.73.63620834.1
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R Merge I (Observed)R-Sym I (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
12.42.5382.50.3170.3172.23.1

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 1KFU PDB ENTRY 1TL92.466.2334375181996.470.200620.197560.25784RANDOM11.827
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]
0.48-0.330.22-0.83
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg35.765
r_dihedral_angle_3_deg17.628
r_dihedral_angle_4_deg13.445
r_dihedral_angle_1_deg6.138
r_scangle_it1.919
r_angle_refined_deg1.237
r_scbond_it1.166
r_mcangle_it0.841
r_mcbond_it0.51
r_nbtor_refined0.299
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg35.765
r_dihedral_angle_3_deg17.628
r_dihedral_angle_4_deg13.445
r_dihedral_angle_1_deg6.138
r_scangle_it1.919
r_angle_refined_deg1.237
r_scbond_it1.166
r_mcangle_it0.841
r_mcbond_it0.51
r_nbtor_refined0.299
r_nbd_refined0.203
r_symmetry_vdw_refined0.187
r_xyhbond_nbd_refined0.144
r_metal_ion_refined0.122
r_symmetry_hbond_refined0.115
r_chiral_restr0.086
r_bond_refined_d0.009
r_gen_planes_refined0.003
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_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 Atoms7396
Nucleic Acid Atoms
Solvent Atoms176
Heterogen Atoms10

Software

Software
Software NamePurpose
MOSFLMdata reduction
SCALAdata scaling
PHASERphasing
REFMACrefinement
PDB_EXTRACTdata extraction