5P53

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 228

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.3
Synchrotron site	BESSY
Beamline	14.3
Temperature [K]	100
Detector technology	CCD
Collection date	2013-04-18
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.262, 72.951, 52.637
Unit cell angles	90.00, 109.33, 90.00

Refinement procedure

Resolution	28.109 - 1.120
R-factor	0.1271
Rwork	0.127
R-free	0.13590
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]	42.710		1.190
High resolution limit [Å]	1.120	3.350	1.120
Rmerge	0.046	0.030	0.324
Rmeas	0.053	0.034	0.411
Total number of observations	455655
Number of reflections	118019	4724	14864
<I/σ(I)>	17.18	48.18	3.21
Completeness [%]	95.3	99.6	74.5
Redundancy	3.86
CC(1/2)	0.999	0.998	0.860

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 228 with the SMILES code CS(=O)(=O)NC1CCCC1