5P3O

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 177

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	2014-08-05
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.207, 72.794, 52.616
Unit cell angles	90.00, 109.24, 90.00

Refinement procedure

Resolution	28.118 - 1.249
R-factor	0.1377
Rwork	0.137
R-free	0.15490
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.198
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]	42.683		1.320
High resolution limit [Å]	1.250	3.730	1.250
Rmerge	0.038	0.019	0.318
Rmeas	0.043	0.022	0.388
Total number of observations	348892
Number of reflections	87290	3331	12864
<I/σ(I)>	20.72	56.94	3.5
Completeness [%]	98.1	97.4	89.7
Redundancy	3.996
CC(1/2)	0.999	0.999	0.883

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 177 with the SMILES code CN1C(C)=C2C=NN=C(Cl)C2=C1C