5P0K

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 67

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)	0.8912
Spacegroup name	P 1 21 1
Unit cell lengths	45.154, 72.811, 52.623
Unit cell angles	90.00, 109.71, 90.00

Refinement procedure

Resolution	27.938 - 1.600
R-factor	0.1485
Rwork	0.146
R-free	0.19180
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.009
RMSD bond angle	1.165
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]	42.508		1.700
High resolution limit [Å]	1.600	4.770	1.600
Rmerge	0.059	0.028	0.346
Rmeas	0.068	0.032	0.405
Total number of observations	166700
Number of reflections	40732	1616	5546
<I/σ(I)>	16.96	38.64	3.79
Completeness [%]	96.2	98.1	81.5
Redundancy	4.092
CC(1/2)	0.998	0.999	0.849

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 67 with the SMILES code OC(=O)C1(CCOCC1)C1=CC=CS1