5LGO

Trypsin inhibitors for the treatment of pancreatitis - cpd 15

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SLS BEAMLINE X10SA
Synchrotron site	SLS
Beamline	X10SA
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-07-14
Detector	DECTRIS PILATUS 2M
Wavelength(s)	1.000
Spacegroup name	P 31 2 1
Unit cell lengths	55.232, 55.232, 106.981
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	35.660 - 1.120
R-factor	0.1757
Rwork	0.175
R-free	0.19660
RMSD bond length	0.010
RMSD bond angle	1.180
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHASER
Refinement software	BUSTER (2.11.4)

Data quality characteristics

	Overall
Low resolution limit [Å]	47.830
High resolution limit [Å]	1.120
Number of reflections	73334
<I/σ(I)>	21.26
Completeness [%]	99.9
Redundancy	5.72

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP		298	Crystallization Reservoir Solution = 25% PEG3350, 0.2 M LISO4, 100 mM Bis-Tris pH 6.5 Crystallization Protein Solution = 60 mg/ml in 1 mM HCl, 10 mM CaCl2. Complex Formation Method = Soaking Crystallization Protocol = equal volumes (0.3ul+0.3ul) Crystallization Method = Vapor diffusion - Hanging drop Crystallization Temperature = 298.0 Cryo Protocol = The crystal was directly flash cooled in the nitrogen gas stream at 100 Kelvin. Crystal from cocrystallization soaked in 1 mM cpd 15 (in DMSO) overnight.