5P8E

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 347

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.2
Synchrotron site	BESSY
Beamline	14.2
Temperature [K]	100
Detector technology	CCD
Collection date	2014-06-04
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.252, 73.004, 52.749
Unit cell angles	90.00, 109.42, 90.00

Refinement procedure

Resolution	29.430 - 1.219
R-factor	0.1326
Rwork	0.132
R-free	0.14980
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.198
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER (2.5.7)
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.677		1.290
High resolution limit [Å]	1.220	3.650	1.220
Rmerge	0.051	0.014	0.625
Rmeas	0.058	0.017	0.718
Total number of observations	392915
Number of reflections	94816	3650	15067
<I/σ(I)>	17.88	73.39	2.18
Completeness [%]	98.6	98.7	97
Redundancy	4.143
CC(1/2)	1.000	1.000	0.737

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	4.6	290	0.1 M ammonium acetate, 0.1 M sodium acetate, 24-30% PEG 4000; crystal obtained by streak-seeding and soaked with 90 mM of fragment 347 with the SMILES code OC1=NC(=NC2=CC=CC=C12)C(=O)NCC1CC1