5P18

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 91

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	CCD
Collection date	2012-11-16
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.430, 73.155, 52.900
Unit cell angles	90.00, 109.67, 90.00

Refinement procedure

Resolution	36.928 - 1.349
R-factor	0.1356
Rwork	0.134
R-free	0.16500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.181
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]	42.779		1.430
High resolution limit [Å]	1.350	4.030	1.350
Rmerge	0.087	0.037	0.679
Rmeas	0.100	0.042	0.780
Total number of observations	299320
Number of reflections	71469	2738	11422
<I/σ(I)>	11.38	34.18	2.11
Completeness [%]	99.6	99.2	98.6
Redundancy	4.188
CC(1/2)	0.998	0.997	0.740

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 91 with the SMILES code OC(=O)C1=CC=C(OC(F)(F)F)C=C1