5P55

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 230

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	2013-04-18
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.269, 73.109, 52.736
Unit cell angles	90.00, 109.40, 90.00

Refinement procedure

Resolution	29.456 - 1.299
R-factor	0.1338
Rwork	0.133
R-free	0.15670
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]	42.697		1.380
High resolution limit [Å]	1.300	3.880	1.300
Rmerge	0.067	0.037	0.599
Rmeas	0.077	0.042	0.684
Total number of observations	331076
Number of reflections	77545	3034	12191
<I/σ(I)>	13.69	36.23	2.55
Completeness [%]	97.2	98.9	94.8
Redundancy	4.269
CC(1/2)	0.998	0.997	0.785

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 230 with the SMILES code OC(=O)C1=C(Br)C(Br)=CS1