5P0Y

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 81

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.1
Synchrotron site	BESSY
Beamline	14.1
Temperature [K]	100
Detector technology	CCD
Collection date	2012-11-16
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.286, 73.166, 52.694
Unit cell angles	90.00, 109.39, 90.00

Refinement procedure

Resolution	29.464 - 1.320
R-factor	0.1341
Rwork	0.133
R-free	0.15290
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]	42.718		1.400
High resolution limit [Å]	1.320	3.940	1.320
Rmerge	0.095	0.068	0.479
Rmeas	0.109	0.078	0.550
Total number of observations	317564
Number of reflections	75485	2925	12018
<I/σ(I)>	9.23	20.25	2.55
Completeness [%]	99.2	99.2	98.2
Redundancy	4.206
CC(1/2)	0.994	0.992	0.821

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 81 with the SMILES code CN(C)C1=CC=CC(=C1)C(=O)NN