5P05

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 52

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	2012-11-16
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.8912
Spacegroup name	P 1 21 1
Unit cell lengths	45.074, 72.960, 52.495
Unit cell angles	90.00, 109.52, 90.00

Refinement procedure

Resolution	36.480 - 1.603
R-factor	0.1598
Rwork	0.158
R-free	0.19680
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.009
RMSD bond angle	1.165
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]	42.484		1.700
High resolution limit [Å]	1.600	4.780	1.600
Rmerge	0.067	0.023	0.632
Rmeas	0.077	0.026	0.745
Total number of observations	165901
Number of reflections	40865	1589	5688
<I/σ(I)>	17.33	47.74	3.1
Completeness [%]	97.1	96.9	84
Redundancy	4.059
CC(1/2)	0.998	0.999	0.876

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 52 with the SMILES code NCC(=O)C1=CC=C(Br)C=C1