5P4C

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 201

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	2014-06-04
Detector	MAR CCD 165 mm
Wavelength(s)	0.895
Spacegroup name	P 1 21 1
Unit cell lengths	45.326, 72.952, 52.793
Unit cell angles	90.00, 109.39, 90.00

Refinement procedure

Resolution	42.755 - 1.257
R-factor	0.1308
Rwork	0.130
R-free	0.14870
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.203
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]	42.756		1.330
High resolution limit [Å]	1.260	3.760	1.260
Rmerge	0.068	0.038	0.564
Rmeas	0.078	0.044	0.649
Total number of observations	363184
Number of reflections	87339	3335	13691
<I/σ(I)>	12.07	32.51	2.34
Completeness [%]	99.2	99	96.5
Redundancy	4.158
CC(1/2)	0.998	0.997	0.779

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 201 with the SMILES code CC1=C(CCO)SC=N1