5P6G

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 277

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	2014-06-04
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.276, 72.898, 52.747
Unit cell angles	90.00, 109.42, 90.00

Refinement procedure

Resolution	34.760 - 1.088
R-factor	0.1304
Rwork	0.130
R-free	0.14400
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.208
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]	42.699		1.150
High resolution limit [Å]	1.090	3.260	1.090
Rmerge	0.051	0.019	0.548
Rmeas	0.059	0.022	0.639
Total number of observations	536079
Number of reflections	134164	5107	21263
<I/σ(I)>	16.64	65.17	2.51
Completeness [%]	99.3	98.7	97.6
Redundancy	3.995
CC(1/2)	0.999	0.999	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 277 with the SMILES code CC1=NN(CC(=O)NC2CC2)C(C)=C1