7EBB

Crystal structure of human pyruvate dehydrogenase kinase 4 in complex with compound 2

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	CLSI BEAMLINE 08ID-1
Synchrotron site	CLSI
Beamline	08ID-1
Temperature [K]	100
Detector technology	CCD
Collection date	2013-09-26
Detector	RAYONIX MX-300
Wavelength(s)	1.0
Spacegroup name	P 1 21 1
Unit cell lengths	70.624, 69.360, 81.283
Unit cell angles	90.00, 100.12, 90.00

Refinement procedure

Resolution	80.020 - 1.900
R-factor	0.1959
Rwork	0.195
R-free	0.21900
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2zkj
RMSD bond length	0.002
RMSD bond angle	0.558
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]	80.020	1.950
High resolution limit [Å]	1.900	1.900
Rmerge	0.052	0.391
Rmeas	0.060	0.453
Rpim	0.030	0.228
Number of reflections	60356	4397
<I/σ(I)>	13.9	3.4
Completeness [%]	99.0	98.2
Redundancy	3.9	3.9
CC(1/2)	0.998	0.900

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