3BWJ

Complex of PKA with the bisubstrate protein kinase inhibitor lead compound Arc-1034

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	VAPOR DIFFUSION, HANGING DROP	6.5	279	Mes-Bis-Tris, LiCl, pH 6.5, VAPOR DIFFUSION, HANGING DROP, temperature 279K

Crystal Properties
Matthews coefficient	Solvent content
2.45	49.74

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 71.188	α = 90
b = 72.632	β = 90
c = 77.221	γ = 90

Symmetry
Space Group	P 21 21 21

Diffraction

Diffraction Experiment
ID #	Crystal ID	Scattering Type	Data Collection Temperature	Detector	Detector Type	Details	Collection Date	Monochromator	Protocol
1	1	x-ray	77	CCD	MAR CCD 165 mm		2006-12-10	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	MPG/DESY, HAMBURG BEAMLINE BW6	1.05	MPG/DESY, HAMBURG	BW6

Data Collection

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	R Sym I (Observed)	Net I Over Average Sigma (I)	Redundancy	Number Reflections (All)	Number Reflections (Observed)	Observed Criterion Sigma (F)	Observed Criterion Sigma (I)	B (Isotropic) From Wilson Plot
1	2.3	52.926	99.9	0.119			17407	18346		1.9	32.7

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	R-Sym I (Observed)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1	2.3	2.36	100		0.387	1.9	1.05	1340

Refinement

Statistics
Diffraction ID	Structure Solution Method	Cross Validation method	Resolution (High)	Resolution (Low)	Number Reflections (Observed)	Number Reflections (R-Free)	Percent Reflections (Observed)	R-Factor (Observed)	R-Work	R-Free	R-Free Selection Details	Mean Isotropic B
X-RAY DIFFRACTION	MOLECULAR REPLACEMENT	THROUGHOUT	2.3	52.926	17407	939	99.87	0.20145	0.19899	0.2493	RANDOM	24.1

Temperature Factor Modeling
Anisotropic B[1][1]	Anisotropic B[1][2]	Anisotropic B[1][3]	Anisotropic B[2][2]	Anisotropic B[2][3]	Anisotropic B[3][3]
-0.03			-0.59		0.62

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	39.111
r_dihedral_angle_4_deg	24.16
r_dihedral_angle_3_deg	18.212
r_dihedral_angle_1_deg	5.984
r_scangle_it	3.843
r_scbond_it	2.491
r_mcangle_it	1.648
r_angle_refined_deg	1.598
r_mcbond_it	1.055
r_symmetry_hbond_refined	0.389

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	39.111
r_dihedral_angle_4_deg	24.16
r_dihedral_angle_3_deg	18.212
r_dihedral_angle_1_deg	5.984
r_scangle_it	3.843
r_scbond_it	2.491
r_mcangle_it	1.648
r_angle_refined_deg	1.598
r_mcbond_it	1.055
r_symmetry_hbond_refined	0.389
r_nbtor_refined	0.308
r_symmetry_vdw_refined	0.228
r_xyhbond_nbd_refined	0.209
r_nbd_refined	0.201
r_chiral_restr	0.115
r_bond_refined_d	0.017
r_gen_planes_refined	0.006

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	2823
Nucleic Acid Atoms
Solvent Atoms	175
Heterogen Atoms	100

Software

Software
Software Name	Purpose
REFMAC	refinement
MOSFLM	data reduction
SCALA	data scaling
AMoRE	phasing

RCSB PDB Core Operations are funded by the National Science Foundation (DBI-1832184), the US Department of Energy (DE-SC0019749), and the National Cancer Institute, National Institute of Allergy and Infectious Diseases, and National Institute of General Medical Sciences of the National Institutes of Health under grant R01GM133198.