5P22

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 120

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	2014-02-15
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.345, 72.938, 52.792
Unit cell angles	90.00, 109.56, 90.00

Refinement procedure

Resolution	28.094 - 1.309
R-factor	0.1337
Rwork	0.133
R-free	0.15320
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.210
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]	42.727		1.390
High resolution limit [Å]	1.310	3.910	1.310
Rmerge	0.055	0.034	0.427
Rmeas	0.064	0.039	0.492
Total number of observations	322250
Number of reflections	77597	2980	12452
<I/σ(I)>	15.87	42.69	3.44
Completeness [%]	99.6	98.8	98.9
Redundancy	4.152
CC(1/2)	0.998	0.998	0.861

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 120 with the SMILES code CC1=CC(NC(=O)CN2CCC3=CC=CC=C23)=NO1