5P2H

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 135

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	45.406, 73.170, 53.013
Unit cell angles	90.00, 109.40, 90.00

Refinement procedure

Resolution	34.886 - 1.621
R-factor	0.1437
Rwork	0.142
R-free	0.17980
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.124
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]	42.827		1.720
High resolution limit [Å]	1.620	4.830	1.620
Rmerge	0.064	0.025	0.500
Rmeas	0.073	0.029	0.576
Total number of observations	170482
Number of reflections	40783	1607	5967
<I/σ(I)>	16.21	46.71	3.08
Completeness [%]	98.1	98.9	89.4
Redundancy	4.18
CC(1/2)	0.999	0.999	0.834

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 135 with the SMILES code FC(F)(F)CN1CCNCC1