5P6M

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 283

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	PIXEL
Collection date	2013-07-18
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 1 21 1
Unit cell lengths	45.330, 72.918, 52.893
Unit cell angles	90.00, 109.57, 90.00

Refinement procedure

Resolution	42.712 - 1.345
R-factor	0.1364
Rwork	0.135
R-free	0.15880
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
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]	42.712		1.430
High resolution limit [Å]	1.340	4.020	1.340
Rmerge	0.067	0.027	0.696
Rmeas	0.078	0.032	0.813
Total number of observations	263278
Number of reflections	68343	2666	10283
<I/σ(I)>	12.54	42.24	1.87
Completeness [%]	94.9	96.4	88.3
Redundancy	3.852
CC(1/2)	0.998	0.998	0.621

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 283 with the SMILES code C[C@@]1(NC(=O)C2=CC=CC=C2N1)C1=CC=NC=C1