5P5B

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 236

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	2013-04-04
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 1 21 1
Unit cell lengths	45.326, 72.966, 52.673
Unit cell angles	90.00, 109.27, 90.00

Refinement procedure

Resolution	42.786 - 1.209
R-factor	0.1308
Rwork	0.130
R-free	0.14420
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.203
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]	42.786		1.280
High resolution limit [Å]	1.210	3.620	1.210
Rmerge	0.052	0.039	0.224
Rmeas	0.060	0.045	0.275
Total number of observations	350067
Number of reflections	96832	3750	14290
<I/σ(I)>	13.67	34.64	3.62
Completeness [%]	98.1	98.7	89.8
Redundancy	3.615
CC(1/2)	0.998	0.996	0.921

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 236 with the SMILES code CNCC1=CC(=CC=C1Cl)[N+]([O-])=O