9FB8

XChem refined PIF1-x0076 complex

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I04-1
Synchrotron site	Diamond
Beamline	I04-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2018-03-08
Detector	DECTRIS PILATUS 6M-F
Wavelength(s)	0.91587
Spacegroup name	C 2 2 21
Unit cell lengths	73.600, 143.714, 77.238
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	27.830 - 1.727
Rwork	0.173
R-free	0.21140
Structure solution method	FOURIER SYNTHESIS
RMSD bond length	0.009
RMSD bond angle	1.896
Data reduction software	DIALS
Data scaling software	DIALS
Phasing software	REFMAC
Refinement software	REFMAC (5.8.0419)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	27.830	1.770
High resolution limit [Å]	1.727	1.730
Number of reflections	43220	3023
<I/σ(I)>	19.5
Completeness [%]	99.6
Redundancy	6.5
CC(1/2)	0.999	0.866

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		277.15	XChem 0.045uls compound (0.5M) in DMSO echo dispensed into crystal drop Drop = 0.3uls protein + 0.3us well +0.001uls seeds. Protein = 25uls 30mgs/ml human PIF1 (206-620) in 10mM Tris pH 7.5, 175mM NaCl, 2%glycerol, 5mM DTT, 0.1mM PMSF + 21uls 10mM Tris, 2.7uls 0.2M MgCl2, 5uls 100mM AMPPNP + 27uls H2O. Well = 4% Glycerol, 27% PEG 2KMME, 0.1M NaAcetate, 0.1M Tris pH8.5. Set up on douglas instruments robot - tray on ice - set-up room temperature - crystallised 4 degrees C.