5P6K

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 281

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)	0.918409
Spacegroup name	P 21 21 21
Unit cell lengths	45.227, 72.786, 104.015
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	42.315 - 1.607
R-factor	0.1663
Rwork	0.163
R-free	0.22590
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.009
RMSD bond angle	1.148
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]	42.316		1.700
High resolution limit [Å]	1.610	4.790	1.610
Rmerge	0.123	0.099	0.315
Rmeas	0.133	0.107	0.351
Total number of observations	270354
Number of reflections	44133	1872	6662
<I/σ(I)>	10.36	13.6	6.17
Completeness [%]	96.9	99.5	92
Redundancy	6.125
CC(1/2)	0.993	0.992	0.902

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 281 with the SMILES code CS(=O)(=O)N[C@H]1CCCNC1