6DUM

ALDH1A1 N121S in complex with 6-{[(3-fluorophenyl)methyl]sulfanyl}-2-(oxetan-3-yl)-5-phenyl-2,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one (compound 13g)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 19-ID
Synchrotron site	APS
Beamline	19-ID
Temperature [K]	100
Detector technology	CCD
Collection date	2017-03-26
Detector	ADSC QUANTUM 315r
Wavelength(s)	0.98
Spacegroup name	P 4 2 2
Unit cell lengths	108.802, 108.802, 82.877
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	50.000 - 2.000
R-factor	0.1971
Rwork	0.194
R-free	0.24860
RMSD bond length	0.010
RMSD bond angle	1.473
Data scaling software	SCALEPACK
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.030
High resolution limit [Å]	2.000	5.430	2.000
Rmerge	0.061	0.045	0.316
Rmeas	0.063	0.047	0.328
Rpim	0.017	0.013	0.090
Total number of observations	418664
Number of reflections	33340
<I/σ(I)>	8.6
Completeness [%]	97.2	99.5	83.6
Redundancy	12.6	11.8	12
CC(1/2)		0.999	0.987

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		300	100 mM Bis-Tris, pH 6.2-6.5, 200 mM sodium chloride, 5 mM ytterbium chloride, 6-11% PEG3350