5P7J

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 316

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	45.452, 73.308, 53.048
Unit cell angles	90.00, 109.57, 90.00

Refinement procedure

Resolution	21.953 - 1.307
R-factor	0.1334
Rwork	0.132
R-free	0.15790
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.176
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]	42.827		1.390
High resolution limit [Å]	1.310	3.910	1.310
Rmerge	0.057	0.027	0.498
Rmeas	0.066	0.031	0.578
Total number of observations	322192
Number of reflections	78624	3021	12344
<I/σ(I)>	14.97	38.31	2.95
Completeness [%]	99.3	99	96.9
Redundancy	4.097
CC(1/2)	0.999	0.999	0.794

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 316 with the SMILES code O[C@H](CN1CCOCC1)C1=CSC2=CC=CC=C12