5P39

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 162

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	2013-04-12
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.285, 72.766, 52.630
Unit cell angles	90.00, 109.38, 90.00

Refinement procedure

Resolution	36.383 - 1.188
R-factor	0.1475
Rwork	0.146
R-free	0.16760
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.198
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]	42.719		1.260
High resolution limit [Å]	1.190	3.550	1.190
Rmerge	0.065	0.031	0.473
Rmeas	0.076	0.036	0.565
Total number of observations	389663
Number of reflections	102282	3933	15746
<I/σ(I)>	14.53	42.22	3.04
Completeness [%]	98.8	99.4	94.3
Redundancy	3.809
CC(1/2)	0.998	0.997	0.831

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 162 with the SMILES code C[C@H](NC(=O)CCC(=O)C1=CC=CS1)C1=CC=CN=C1