5P23

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 121

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	45.504, 73.092, 53.061
Unit cell angles	90.00, 109.41, 90.00

Refinement procedure

Resolution	42.917 - 1.713
R-factor	0.1514
Rwork	0.149
R-free	0.19970
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.009
RMSD bond angle	1.125
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]	42.918		1.820
High resolution limit [Å]	1.710	5.110	1.710
Rmerge	0.053	0.022	0.376
Rmeas	0.061	0.025	0.445
Total number of observations	139054
Number of reflections	34222	1380	4766
<I/σ(I)>	22.75	55.81	5.26
Completeness [%]	96.9	99.6	83.7
Redundancy	4.063
CC(1/2)	0.999	0.999	0.920

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 121 with the SMILES code CC1(C)N[C@@H](CS1)C(O)=O