5P61

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 262

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.1
Synchrotron site	BESSY
Beamline	14.1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-07-18
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 1 21 1
Unit cell lengths	45.294, 73.052, 52.718
Unit cell angles	90.00, 109.34, 90.00

Refinement procedure

Resolution	36.889 - 1.089
R-factor	0.1272
Rwork	0.127
R-free	0.14050
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.217
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]	42.739		1.160
High resolution limit [Å]	1.090	3.260	1.090
Rmerge	0.038	0.021	0.428
Rmeas	0.044	0.025	0.517
Total number of observations	469689
Number of reflections	134311	5144	21475
<I/σ(I)>	15.94	57.05	2.61
Completeness [%]	99.5	99.5	98.7
Redundancy	3.497
CC(1/2)	0.999	0.999	0.821

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 262 with the SMILES code CC(=O)C1=C(C)NC(C(=O)N2CCC2)=C1C