5OZ3

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 14

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	2012-09-04
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.9184
Spacegroup name	P 1 21 1
Unit cell lengths	45.599, 72.823, 52.732
Unit cell angles	90.00, 108.86, 90.00

Refinement procedure

Resolution	43.150 - 1.754
R-factor	0.159
Rwork	0.156
R-free	0.21660
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.010
RMSD bond angle	1.193
Data reduction software	HKL-2000
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]	50.000	50.000	1.780
High resolution limit [Å]	1.750	4.750	1.750
Rmerge	0.080	0.037	0.437
Total number of observations	125888
Number of reflections	31788
<I/σ(I)>	11.9
Completeness [%]	97.8	98.9	95.9
Redundancy	4	4	4

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 14 with the SMILES code CNC(=S)NC1=CC=C(Br)C=C1Cl