5P1M

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 105

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	2013-01-23
Detector	MAR CCD 165 mm
Wavelength(s)	0.8946
Spacegroup name	P 1 21 1
Unit cell lengths	45.264, 72.975, 52.601
Unit cell angles	90.00, 109.30, 90.00

Refinement procedure

Resolution	42.720 - 1.599
R-factor	0.1398
Rwork	0.137
R-free	0.18820
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.129
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]	42.721		1.700
High resolution limit [Å]	1.600	4.770	1.600
Rmerge	0.068	0.024	0.485
Rmeas	0.079	0.028	0.575
Total number of observations	168542
Number of reflections	41986	1645	6674
<I/σ(I)>	16.72	47.33	2.52
Completeness [%]	98.2	98.9	96.8
Redundancy	4.014
CC(1/2)	0.998	0.999	0.767

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 105 with the SMILES code CCCC1=C(C)SC(=C1)C(=O)NN