5P17

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 90

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	2015-07-17
Detector	MAR CCD 165 mm
Wavelength(s)	0.895
Spacegroup name	P 1 21 1
Unit cell lengths	45.167, 72.713, 52.499
Unit cell angles	90.00, 109.03, 90.00

Refinement procedure

Resolution	28.146 - 1.399
R-factor	0.1432
Rwork	0.142
R-free	0.17100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.152
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]	42.698		1.480
High resolution limit [Å]	1.400	4.180	1.400
Rmerge	0.065	0.023	0.689
Rmeas	0.074	0.027	0.794
Total number of observations	262966
Number of reflections	62934	2435	9986
<I/σ(I)>	15.86	52.42	2.23
Completeness [%]	99.5	99.3	98.5
Redundancy	4.178
CC(1/2)	0.999	0.999	0.727

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 90 with the SMILES code ClCC(=O)NC1CCCC1