5P5S

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 253

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	2014-08-05
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 1 21 1
Unit cell lengths	45.330, 72.945, 52.817
Unit cell angles	90.00, 109.48, 90.00

Refinement procedure

Resolution	28.125 - 1.139
R-factor	0.1314
Rwork	0.131
R-free	0.14480
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.201
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]	42.736		1.210
High resolution limit [Å]	1.140	3.410	1.140
Rmerge	0.041	0.016	0.497
Rmeas	0.048	0.018	0.584
Total number of observations	433726
Number of reflections	117466	4488	18733
<I/σ(I)>	16.67	72.04	2.38
Completeness [%]	99.5	98.9	98.5
Redundancy	3.692
CC(1/2)	1.000	0.999	0.783

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 253 with the SMILES code C[C@@H](CN)N1C[C@H](C)O[C@H](C)C1