4GBK

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	77.500, 77.500, 37.600
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	38.750 - 2.400
R-factor	0.2011
Rwork	0.198
R-free	0.26590
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1zeh
RMSD bond length	0.018
RMSD bond angle	2.029
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]	38.750	32.803	2.530
High resolution limit [Å]	2.400	7.590	2.400
Rmerge		0.011	0.011
Total number of observations		243	1245
Number of reflections	3189
<I/σ(I)>	4.2	4.8	0.6
Completeness [%]	96.9	82.1	98.7
Redundancy	2.8	2.9	2.7

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