5P38

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 161

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	2013-04-12
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.300, 72.892, 52.628
Unit cell angles	90.00, 109.49, 90.00

Refinement procedure

Resolution	39.540 - 1.289
R-factor	0.138
Rwork	0.137
R-free	0.16220
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.191
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]	42.704		1.370
High resolution limit [Å]	1.290	3.850	1.290
Rmerge	0.058	0.024	0.498
Rmeas	0.067	0.028	0.575
Total number of observations	311317
Number of reflections	78918	3086	12426
<I/σ(I)>	17.39	53.56	3.38
Completeness [%]	97.2	99	95.2
Redundancy	3.944
CC(1/2)	0.999	0.999	0.825

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 161 with the SMILES code COC(=O)C1=C(C)NC(=C1C)C1=C(C)SC(N)=N1