5P0I

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 65

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	CCD
Collection date	2012-11-16
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.8912
Spacegroup name	P 1 21 1
Unit cell lengths	45.103, 72.828, 52.546
Unit cell angles	90.00, 109.42, 90.00

Refinement procedure

Resolution	25.395 - 1.149
R-factor	0.1296
Rwork	0.129
R-free	0.14590
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.242
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]	42.538		1.220
High resolution limit [Å]	1.150	3.440	1.150
Rmerge	0.048	0.020	0.462
Rmeas	0.055	0.023	0.539
Total number of observations	452690
Number of reflections	111642	4254	16491
<I/σ(I)>	18.75	57.91	3.36
Completeness [%]	98.0	97.6	89.6
Redundancy	4.054
CC(1/2)	0.999	0.999	0.837

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 65 with the SMILES code CC1=NC(CCN)=CS1