4GBL

Crystal structure of aspart insulin at pH 8.5

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	LNLS BEAMLINE W01B-MX2
Synchrotron site	LNLS
Beamline	W01B-MX2
Temperature [K]	100
Detector technology	CCD
Collection date	2011-10-17
Detector	MARMOSAIC 225 mm CCD
Spacegroup name	H 3
Unit cell lengths	78.570, 78.570, 37.730
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	39.285 - 2.500
R-factor	0.2042
Rwork	0.200
R-free	0.26180
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1zeh
RMSD bond length	0.016
RMSD bond angle	1.844
Data reduction software	MOSFLM
Data scaling software	SCALA (3.3.16)
Phasing software	MOLREP
Refinement software	REFMAC

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	39.285	25.267	2.640
High resolution limit [Å]	2.500	7.910	2.500
Rmerge		0.113	0.807
Total number of observations		183	874
Number of reflections	2950
<I/σ(I)>	3.1	4.8	0.8
Completeness [%]	98.3	89.9	97.4
Redundancy	2.2	2.2	2.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8.5	293	2 uL mother liquor (0.1 M Tris, pH 8.5, 1.5 M ammonium sulfate, 12% v/v glycerol) + 2 uL protein (aspart insulin 100 U/mL), VAPOR DIFFUSION, HANGING DROP, temperature 293K