5P6C

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 273

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	2013-07-18
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.581, 72.959, 53.043
Unit cell angles	90.00, 109.35, 90.00

Refinement procedure

Resolution	43.007 - 1.339
R-factor	0.1328
Rwork	0.132
R-free	0.15630
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.151
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]	43.007		1.420
High resolution limit [Å]	1.340	4.000	1.340
Rmerge	0.049	0.022	0.488
Rmeas	0.058	0.026	0.576
Total number of observations	264916
Number of reflections	72919	2808	11390
<I/σ(I)>	15.27	47.72	2.25
Completeness [%]	99.0	99	96.2
Redundancy	3.633
CC(1/2)	0.999	0.999	0.789

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 273 with the SMILES code CN(C)C(=O)C[C@@H]1N(C=CC2=CC=CC=C12)C(C)=O