5P4S

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 217

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	2013-04-18
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.342, 73.000, 52.845
Unit cell angles	90.00, 109.50, 90.00

Refinement procedure

Resolution	36.885 - 1.308
R-factor	0.1333
Rwork	0.132
R-free	0.15560
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.178
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]	42.742		1.390
High resolution limit [Å]	1.310	3.910	1.310
Rmerge	0.060	0.022	0.639
Rmeas	0.068	0.026	0.739
Total number of observations	323150
Number of reflections	77905	2997	12464
<I/σ(I)>	15.35	51.74	2.17
Completeness [%]	99.5	99	98.5
Redundancy	4.148
CC(1/2)	0.999	0.999	0.727

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 217 with the SMILES code CCN1N=C(C)C(Br)=C1C(O)=O