5BTS

Structural and biophysical characterization of a covalent insulin dimer formed during storage of neutral formulation of human insulin

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU MICROMAX-007 HF
Temperature [K]	100
Detector technology	CCD
Collection date	2014-09-10
Detector	MAR CCD 165 mm
Wavelength(s)	1.5418
Spacegroup name	I 21 3
Unit cell lengths	78.392, 78.392, 78.392
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	39.196 - 1.770
R-factor	0.162
Rwork	0.157
R-free	0.20590
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.010
RMSD bond angle	1.084
Data reduction software	HKL-2000
Data scaling software	SCALEPACK
Phasing software	PHASER
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	1.800
High resolution limit [Å]	1.770	4.800	1.770
Rmerge	0.150	0.105	0.489
Rmeas	0.153	0.107	0.519
Rpim	0.029	0.020	0.166
Total number of observations	215847
Number of reflections	8003
<I/σ(I)>	9.4		3.3
Completeness [%]	99.8	100	95.8
Redundancy	27	27.6	9
CC(1/2)		0.998	0.821

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.5	291	0.2 M Ammonium sulfate, 0.1 M Hepes, 25% w/v PEG3350