5P25

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 123

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	2014-06-04
Detector	MAR CCD 165 mm
Wavelength(s)	0.895
Spacegroup name	P 1 21 1
Unit cell lengths	45.236, 72.899, 52.622
Unit cell angles	90.00, 109.28, 90.00

Refinement procedure

Resolution	28.115 - 1.259
R-factor	0.1339
Rwork	0.133
R-free	0.15920
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.201
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]	42.700		1.340
High resolution limit [Å]	1.260	3.770	1.260
Rmerge	0.066	0.023	0.688
Rmeas	0.075	0.027	0.792
Total number of observations	362402
Number of reflections	86760	3310	13897
<I/σ(I)>	14.31	51.06	2.08
Completeness [%]	99.7	99.3	99.2
Redundancy	4.177
CC(1/2)	0.999	0.999	0.722

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 123 with the SMILES code COC(=O)C1=CC(Br)=CC=C1N