5P4R

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 216

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.2
Synchrotron site	BESSY
Beamline	14.2
Temperature [K]	100
Detector technology	CCD
Collection date	2014-06-04
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.224, 72.957, 52.636
Unit cell angles	90.00, 109.53, 90.00

Refinement procedure

Resolution	29.389 - 1.130
R-factor	0.1482
Rwork	0.147
R-free	0.16530
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.177
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]	42.623		1.200
High resolution limit [Å]	1.130	3.380	1.130
Rmerge	0.048	0.019	0.451
Rmeas	0.055	0.022	0.523
Total number of observations	473107
Number of reflections	114817	4528	17169
<I/σ(I)>	17.35	59.59	2.96
Completeness [%]	95.4	98	88.5
Redundancy	4.12
CC(1/2)	0.999	0.999	0.828

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 216 with the SMILES code NC(=N)C1=CC=C(C=C1)C(F)(F)F