5P52

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 227

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	45.342, 73.490, 53.026
Unit cell angles	90.00, 109.56, 90.00

Refinement procedure

Resolution	29.602 - 1.270
R-factor	0.1353
Rwork	0.134
R-free	0.15790
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.202
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]	42.726		1.350
High resolution limit [Å]	1.270	3.800	1.270
Rmerge	0.048	0.023	0.483
Rmeas	0.055	0.026	0.552
Total number of observations	357018
Number of reflections	84492	3286	13403
<I/σ(I)>	18.82	56.38	3.22
Completeness [%]	97.8	99.2	96.5
Redundancy	4.225
CC(1/2)	0.999	0.999	0.834

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 227 with the SMILES code OC(=O)C1=CC=C(CBr)C=C1