5P50

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 225

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	2013-04-18
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.253, 73.051, 52.627
Unit cell angles	90.00, 109.26, 90.00

Refinement procedure

Resolution	29.428 - 1.119
R-factor	0.1227
Rwork	0.122
R-free	0.13640
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.216
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]	42.719		1.190
High resolution limit [Å]	1.120	3.350	1.120
Rmerge	0.037	0.019	0.292
Rmeas	0.043	0.022	0.373
Total number of observations	457321
Number of reflections	118310	4736	14872
<I/σ(I)>	20.67	65.79	3.46
Completeness [%]	95.2	99.6	74.2
Redundancy	3.865
CC(1/2)	0.999	0.999	0.874

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 225 with the SMILES code NNC(=O)C1=CC(Br)=C(Br)S1