5P56

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 231

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	45.182, 73.065, 52.676
Unit cell angles	90.00, 109.45, 90.00

Refinement procedure

Resolution	28.049 - 1.499
R-factor	0.1404
Rwork	0.138
R-free	0.17810
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.172
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]	42.604		1.590
High resolution limit [Å]	1.500	4.470	1.500
Rmerge	0.073	0.039	0.485
Rmeas	0.084	0.045	0.559
Total number of observations	215958
Number of reflections	51590	1990	8259
<I/σ(I)>	13.32	34.48	2.99
Completeness [%]	99.5	98.7	99.1
Redundancy	4.186
CC(1/2)	0.998	0.997	0.815

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 231 with the SMILES code CC1=CN2C[C@@H](O)CN=C2C=C1