5P1Y

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 117

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	2013-01-23
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.295, 73.085, 52.802
Unit cell angles	90.00, 109.52, 90.00

Refinement procedure

Resolution	22.272 - 1.518
R-factor	0.1601
Rwork	0.158
R-free	0.19650
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.009
RMSD bond angle	1.190
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]	42.690		1.610
High resolution limit [Å]	1.520	4.530	1.520
Rmerge	0.102	0.048	0.640
Rmeas	0.118	0.056	0.731
Total number of observations	204833
Number of reflections	48823	1884	7647
<I/σ(I)>	10.3	26.94	2.34
Completeness [%]	97.2	96.9	94.4
Redundancy	4.195
CC(1/2)	0.996	0.994	0.780

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 117 with the SMILES code N\C(=N/O)C1=CC(Br)=CC=C1