5P01

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 48

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	CCD
Collection date	2012-09-04
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.614, 72.433, 52.747
Unit cell angles	90.00, 108.94, 90.00

Refinement procedure

Resolution	43.144 - 1.514
R-factor	0.1429
Rwork	0.141
R-free	0.17760
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.184
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]	43.143		1.610
High resolution limit [Å]	1.510	4.520	1.510
Rmerge	0.056	0.020	0.503
Rmeas	0.064	0.022	0.577
Total number of observations	204697
Number of reflections	48966	1948	6641
<I/σ(I)>	18.99	57.29	2.99
Completeness [%]	96.9	99.3	82.1
Redundancy	4.18
CC(1/2)	0.999	0.999	0.832

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 48 with the SMILES code ClC1=CC=C(NC(=O)C(=O)N2CCCC2)N=C1