5P1S

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 111

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	2014-02-15
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.252, 73.153, 52.653
Unit cell angles	90.00, 109.32, 90.00

Refinement procedure

Resolution	39.481 - 1.319
R-factor	0.1304
Rwork	0.129
R-free	0.15320
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.220
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]	42.703		1.400
High resolution limit [Å]	1.320	3.940	1.320
Rmerge	0.050	0.020	0.427
Rmeas	0.057	0.023	0.488
Total number of observations	316276
Number of reflections	74424	2914	11683
<I/σ(I)>	18.04	52.33	3.33
Completeness [%]	97.7	98.7	95.5
Redundancy	4.249
CC(1/2)	0.999	0.999	0.879

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 111 with the SMILES code OC(=O)C1CCN(CC1)C(=O)CCl