5M4P

Application of Off-Rate Screening in the Identification of Novel Pan-Isoform Inhibitors of Pyruvate Dehydrogenase Kinase

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU RUH3R
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2011-02-10
Detector	RIGAKU RAXIS IV++
Wavelength(s)	1.5412
Spacegroup name	P 64
Unit cell lengths	109.442, 109.442, 84.515
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	20.000 - 2.300
R-factor	0.20218
Rwork	0.200
R-free	0.25178
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2bu8
RMSD bond length	0.016
RMSD bond angle	1.858
Data reduction software	d*TREK
Data scaling software	d*TREK
Phasing software	AMoRE
Refinement software	REFMAC (5.8.0135)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	29.590	2.380
High resolution limit [Å]	2.300	2.300
Rmerge	0.090	0.541
Number of reflections	25546
<I/σ(I)>	7.1	1.5
Completeness [%]	99.4	99
Redundancy	3.65	3.53

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION	5.8	277	0.1 M SODIUM ACETATE PH 5.8 0.125 M MAGNESIUM CHLORIDE 6% ISOPROPANOL