5P7S

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 325

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	2014-01-22
Detector	MAR CCD 165 mm
Wavelength(s)	0.895
Spacegroup name	P 1 21 1
Unit cell lengths	45.282, 72.988, 52.757
Unit cell angles	90.00, 109.54, 90.00

Refinement procedure

Resolution	21.853 - 1.189
R-factor	0.1315
Rwork	0.131
R-free	0.15100
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.183
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]	42.673		1.260
High resolution limit [Å]	1.190	3.560	1.190
Rmerge	0.051	0.018	0.539
Rmeas	0.058	0.021	0.629
Total number of observations	420489
Number of reflections	102006	3938	15689
<I/σ(I)>	16.95	65.17	2.39
Completeness [%]	98.4	99.3	93.7
Redundancy	4.122
CC(1/2)	0.999	0.999	0.772

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 325 with the SMILES code CN(C)C(=O)CN1CCNCC1