5P7I

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 315

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	45.251, 73.203, 52.936
Unit cell angles	90.00, 109.57, 90.00

Refinement procedure

Resolution	22.518 - 1.187
R-factor	0.1342
Rwork	0.133
R-free	0.15180
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.203
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]	42.636		1.260
High resolution limit [Å]	1.190	3.550	1.190
Rmerge	0.061	0.032	0.572
Rmeas	0.069	0.036	0.656
Total number of observations	428261
Number of reflections	101905	3982	15562
<I/σ(I)>	12.85	37.46	2.41
Completeness [%]	97.3	99.2	92.1
Redundancy	4.202
CC(1/2)	0.999	0.998	0.811

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 315 with the SMILES code O=C1NC=NC2=C1N=C(N2)N1CCCCC1