7EAT

Crystal structure of human pyruvate dehydrogenase kinase 4 in complex with compound 1

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	PHOTON FACTORY BEAMLINE BL-17A
Synchrotron site	Photon Factory
Beamline	BL-17A
Temperature [K]	100
Detector technology	CCD
Collection date	2013-10-29
Detector	ADSC QUANTUM 270
Wavelength(s)	1.0
Spacegroup name	P 1 21 1
Unit cell lengths	70.363, 67.979, 78.945
Unit cell angles	90.00, 101.11, 90.00

Refinement procedure

Resolution	77.470 - 2.100
R-factor	0.1957
Rwork	0.194
R-free	0.22830
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2zkj
RMSD bond length	0.002
RMSD bond angle	0.468
Data reduction software	DIALS
Data scaling software	Aimless
Phasing software	MOLREP
Refinement software	PHENIX (1.19rc3_4028)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	77.470	3.800
High resolution limit [Å]	2.100	2.100
Rmerge	0.069	0.258
Rmeas	0.081	0.301
Rpim	0.042	0.154
Number of reflections	42561	3104
<I/σ(I)>	9.7	3.1
Completeness [%]	99.4	99.2
Redundancy	3.7	3.8
CC(1/2)	0.996	0.926

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	295.15	50 mM KHPO4 pH 7.5, 1.7 M ammonium sulfate and 4% (v/v) PEG400, 5 mM ADP