5P3A

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 163

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.1
Synchrotron site	BESSY
Beamline	14.1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-04-04
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 1 21 1
Unit cell lengths	45.271, 73.387, 52.723
Unit cell angles	90.00, 109.22, 90.00

Refinement procedure

Resolution	42.748 - 1.177
R-factor	0.1376
Rwork	0.137
R-free	0.15530
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.205
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]	42.748		1.250
High resolution limit [Å]	1.180	3.520	1.180
Rmerge	0.040	0.021	0.343
Rmeas	0.047	0.025	0.440
Total number of observations	360358
Number of reflections	102585	4102	13022
<I/σ(I)>	16.12	54.79	2.33
Completeness [%]	95.4	99.4	75.1
Redundancy	3.512
CC(1/2)	0.999	0.999	0.812

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 163 with the SMILES code CN(CC(=O)NC1CC1)S(=O)(=O)C1=CC=C(Br)S1