4GBI

Crystal structure of aspart insulin at pH 6.5

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	LNLS BEAMLINE D03B-MX1
Synchrotron site	LNLS
Beamline	D03B-MX1
Temperature [K]	100
Detector technology	CCD
Collection date	2011-10-17
Detector	MAR CCD 165 mm
Spacegroup name	H 3
Unit cell lengths	78.290, 78.290, 36.910
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	39.145 - 2.502
R-factor	0.1578
Rwork	0.152
R-free	0.20230
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1zeh
RMSD bond length	0.018
RMSD bond angle	1.954
Data reduction software	MOSFLM
Data scaling software	SCALA (3.3.20)
Phasing software	MOLREP
Refinement software	REFMAC

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	39.145	24.968	2.640
High resolution limit [Å]	2.502	7.910	2.502
Rmerge		0.041	0.470
Total number of observations		109	636
Number of reflections	2607
<I/σ(I)>	8.8	13.6	1
Completeness [%]	89.3	63.8	92.5
Redundancy	1.7	1.8	1.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.5	293	2 uL mother liquor (0.1 M MES, pH 6.5, 1.6 M magnesium sulfate heptahydrate) + 2 uL protein (aspart insulin, 100 U/mL), VAPOR DIFFUSION, HANGING DROP, temperature 293K