5P5X

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 258

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	45.269, 73.013, 52.729
Unit cell angles	90.00, 109.38, 90.00

Refinement procedure

Resolution	36.507 - 1.069
R-factor	0.1245
Rwork	0.124
R-free	0.13690
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.197
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]	42.703		1.130
High resolution limit [Å]	1.070	3.200	1.070
Rmerge	0.029	0.013	0.437
Rmeas	0.034	0.015	0.523
Total number of observations	481138
Number of reflections	135944	5376	20586
<I/σ(I)>	20.99	85.05	2.52
Completeness [%]	95.4	99	89.4
Redundancy	3.539
CC(1/2)	1.000	1.000	0.822

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 258 with the SMILES code CC(C)N1N=CC2=C1N=CC(=C2)C(=O)NCC1CC1