5P13

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 86

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.3
Synchrotron site	BESSY
Beamline	14.3
Temperature [K]	100
Detector technology	CCD
Collection date	2014-02-15
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.296, 72.923, 52.797
Unit cell angles	90.00, 109.55, 90.00

Refinement procedure

Resolution	39.601 - 1.399
R-factor	0.1463
Rwork	0.145
R-free	0.17500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.159
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]	42.684		1.480
High resolution limit [Å]	1.400	4.180	1.400
Rmerge	0.085	0.046	0.546
Rmeas	0.097	0.054	0.624
Total number of observations	263535
Number of reflections	61968	2414	9722
<I/σ(I)>	12.72	31.2	3.33
Completeness [%]	97.0	97.3	94.6
Redundancy	4.252
CC(1/2)	0.997	0.995	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 86 with the SMILES code FC1=CC(NC(=O)CCl)=CC=C1