4ZAR

Crystal Structure of Proteinase K from Engyodontium albuminhibited by METHOXYSUCCINYL-ALA-ALA-PRO-PHE-CHLOROMETHYL KETONE at 1.15 A resolution

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	VAPOR DIFFUSION, HANGING DROP	7.5	277	Ammonium Sulfate , Tris HCL, calcium chloride

Crystal Properties
Matthews coefficient	Solvent content
1.97	37.55

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 67.85	α = 90
b = 67.85	β = 90
c = 102.51	γ = 90

Symmetry
Space Group	P 43 21 2

Diffraction

Diffraction Experiment
ID #	Crystal ID	Scattering Type	Data Collection Temperature	Detector	Detector Type	Details	Collection Date	Monochromator	Protocol
1	1	x-ray	100	PIXEL	DECTRIS PILATUS 6M		2014-04-04	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	APS BEAMLINE 24-ID-C	0.979200	APS	24-ID-C

Data Collection

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	R Merge I (Observed)	Rrim I (All)	Net I Over Average Sigma (I)	Redundancy	Number Reflections (All)	Number Reflections (Observed)	Observed Criterion Sigma (F)	Observed Criterion Sigma (I)	B (Isotropic) From Wilson Plot
1	1.15	56.6	97.2	0.067	0.07	18.82	12.2		82922		-3	16.018

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	R Merge I (Observed)	Rrim I (All)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1	1.15	1.18	74.4		0.591	0.63	3.26

Refinement

Statistics
Diffraction ID	Structure Solution Method	Cross Validation method	Starting model	Resolution (High)	Resolution (Low)	Number Reflections (Observed)	Number Reflections (R-Free)	Percent Reflections (Observed)	R-Factor (Observed)	R-Work	R-Free	R-Free Selection Details	Mean Isotropic B
X-RAY DIFFRACTION	FOURIER SYNTHESIS	THROUGHOUT	3PRK	1.15	56.58	74629	8293	97.17	0.1124	0.1099	0.1345	RANDOM	14.417

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]
-0.1			-0.1		0.2

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	37.28
r_sphericity_free	25.404
r_dihedral_angle_4_deg	18.509
r_dihedral_angle_3_deg	11.252
r_dihedral_angle_1_deg	9.525
r_sphericity_bonded	8.843
r_rigid_bond_restr	4.257
r_angle_refined_deg	1.766
r_mcangle_it	1.376
r_mcbond_other	1.323

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	37.28
r_sphericity_free	25.404
r_dihedral_angle_4_deg	18.509
r_dihedral_angle_3_deg	11.252
r_dihedral_angle_1_deg	9.525
r_sphericity_bonded	8.843
r_rigid_bond_restr	4.257
r_angle_refined_deg	1.766
r_mcangle_it	1.376
r_mcbond_other	1.323
r_mcbond_it	1.322
r_angle_other_deg	0.9
r_chiral_restr	0.118
r_bond_refined_d	0.026
r_gen_planes_refined	0.009
r_bond_other_d	0.001
r_gen_planes_other	0.001

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	2066
Nucleic Acid Atoms
Solvent Atoms	318
Heterogen Atoms	2

Software

Software
Software Name	Purpose
XSCALE	data scaling
REFMAC	refinement
PDB_EXTRACT	data extraction
XDS	data reduction
REFMAC	phasing

RCSB PDB Core Operations are funded by the U.S. National Science Foundation (DBI-2321666), the US Department of Energy (DE-SC0019749), and the National Cancer Institute, National Institute of Allergy and Infectious Diseases, and National Institute of General Medical Sciences of the National Institutes of Health under grant R01GM133198.