5P15

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 88

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	45.334, 73.049, 52.854
Unit cell angles	90.00, 109.59, 90.00

Refinement procedure

Resolution	34.845 - 1.410
R-factor	0.1297
Rwork	0.128
R-free	0.16090
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.167
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]	42.710		1.500
High resolution limit [Å]	1.410	4.210	1.410
Rmerge	0.065	0.035	0.416
Rmeas	0.074	0.041	0.483
Total number of observations	249063
Number of reflections	59194	2402	7532
<I/σ(I)>	14.67	36.04	2.87
Completeness [%]	94.6	99	75
Redundancy	4.207
CC(1/2)	0.998	0.997	0.827

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 88 with the SMILES code CN(C)C1=CC=C(NC(=O)CCl)C=C1