5P26

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 124

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	2013-01-23
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.267, 73.310, 52.856
Unit cell angles	90.00, 109.25, 90.00

Refinement procedure

Resolution	26.314 - 1.411
R-factor	0.1324
Rwork	0.131
R-free	0.15380
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.174
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]	42.737		1.500
High resolution limit [Å]	1.410	4.210	1.410
Rmerge	0.066	0.024	0.479
Rmeas	0.075	0.027	0.553
Total number of observations	254528
Number of reflections	61416	2406	8940
<I/σ(I)>	15.75	49.25	3.11
Completeness [%]	97.9	99	88.6
Redundancy	4.144
CC(1/2)	0.999	0.999	0.815

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 124 with the SMILES code CC1=NN(CC(=O)NC2CC2)C(C)=C1[N+]([O-])=O