5P04

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 51

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	45.107, 72.812, 52.495
Unit cell angles	90.00, 109.50, 90.00

Refinement procedure

Resolution	42.520 - 1.669
R-factor	0.1471
Rwork	0.144
R-free	0.19760
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.130
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]	42.520		1.770
High resolution limit [Å]	1.670	4.980	1.670
Rmerge	0.095	0.034	0.478
Rmeas	0.108	0.039	0.548
Total number of observations	154234
Number of reflections	37024	1429	5927
<I/σ(I)>	15.28	36.63	3.37
Completeness [%]	99.3	98.3	99
Redundancy	4.165
CC(1/2)	0.997	0.998	0.841

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 51 with the SMILES code O=C1NC2=CC=C(NCC3=CC=CC=N3)C=C2N1