9R4A

Spitrobot-2 advances time-resolvedcryo-trapping crystallography to under 25 ms: Human insulin, pH 4.5 (50 ms soaking)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE MASSIF-3
Synchrotron site	ESRF
Beamline	MASSIF-3
Temperature [K]	100
Detector technology	PIXEL
Collection date	2025-02-08
Detector	DECTRIS EIGER X 4M
Wavelength(s)	0.968
Spacegroup name	I 21 3
Unit cell lengths	78.345, 78.345, 78.345
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	39.173 - 1.450
R-factor	0.17167
Rwork	0.170
R-free	0.19565
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.014
RMSD bond angle	2.051
Data reduction software	XDS
Data scaling software	Aimless
Phasing software	PHASER
Refinement software	REFMAC (5.8.0430)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	39.173	1.549
High resolution limit [Å]	1.439	1.439
Number of reflections	12209	610
<I/σ(I)>	8.2
Completeness [%]	94.4
Redundancy	5.97
CC(1/2)	0.994	0.387

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	BATCH MODE	9	293	1.0 M sodium/potassium phosphate, pH 9.0 & crystal soaking in pH 4.5 for 50 ms