5P24

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 122

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	2013-01-23
Detector	MAR CCD 165 mm
Wavelength(s)	0.8946
Spacegroup name	P 1 21 1
Unit cell lengths	45.277, 72.989, 52.560
Unit cell angles	90.00, 109.18, 90.00

Refinement procedure

Resolution	29.404 - 1.709
R-factor	0.1439
Rwork	0.141
R-free	0.19480
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.009
RMSD bond angle	1.136
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]	42.764		1.810
High resolution limit [Å]	1.710	5.090	1.710
Rmerge	0.064	0.026	0.344
Rmeas	0.073	0.030	0.402
Total number of observations	140410
Number of reflections	34311	1361	4993
<I/σ(I)>	28.37	54.51	8.34
Completeness [%]	97.7	99.1	87.7
Redundancy	4.092
CC(1/2)	0.998	0.999	0.903

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 122 with the SMILES code CNC1=NC(CC(C)=O)=NS1