7M3Y

Structure of TIM-3 in complex with 8-chloro-2-methyl-9-(3-mehtylpyridin-4-yl)-[1,2,4]triazolo[1,5-c]quinazolin-5(6H)-one (compound 22)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 21-ID-F
Synchrotron site	APS
Beamline	21-ID-F
Temperature [K]	100
Detector technology	CCD
Collection date	2018-07-19
Detector	RAYONIX MX300HE
Wavelength(s)	0.987
Spacegroup name	C 2 2 21
Unit cell lengths	46.958, 85.343, 53.697
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	26.850 - 1.690
R-factor	0.1882
Rwork	0.187
R-free	0.21310
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	5f71
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER (2.8.1)
Refinement software	PHENIX (1.19.1_4122)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	30.000	30.000	1.720
High resolution limit [Å]	1.690	4.580	1.690
Rmerge	0.097	0.037	0.763
Rmeas	0.104	0.040	0.817
Rpim	0.036	0.015	0.288
Total number of observations	99824
Number of reflections	12404	689	607
<I/σ(I)>	6.3
Completeness [%]	100.0	99.9	100
Redundancy	8	7.3	7.9
CC(1/2)		0.999	0.766

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		291	0.8 M sodium tartrate dibasic dihydrate, 0.1 M HEPES pH 6.8-8.2, and 10 mM CaCl2