5P2A

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 128

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.2
Synchrotron site	BESSY
Beamline	14.2
Temperature [K]	100
Detector technology	CCD
Collection date	2013-01-23
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.294, 72.888, 52.610
Unit cell angles	90.00, 109.25, 90.00

Refinement procedure

Resolution	24.834 - 1.373
R-factor	0.1757
Rwork	0.174
R-free	0.20510
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.190
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]	42.761		1.460
High resolution limit [Å]	1.370	4.100	1.370
Rmerge	0.084	0.034	0.653
Rmeas	0.097	0.039	0.745
Total number of observations	267885
Number of reflections	64618	2536	9566
<I/σ(I)>	12.12	35.24	2.34
Completeness [%]	96.0	98	88.1
Redundancy	4.145
CC(1/2)	0.997	0.997	0.757

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 128 with the SMILES code CC[C@H](Br)C(=O)NC1=NOC(C)=C1