6H0U

X-RAY DIFFRACTION

Initial Refinement Model(s)
Type	Source	Accession Code	Details
experimental model	PDB	1Q5K

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	VAPOR DIFFUSION, SITTING DROP	7	293	GSK3beta(35-386) aliquots were concentrated to 4.4 mg/ml and used for crystallization trials. GSK3b-inhibitor co-crystals were grown using the sitting drop vapor diffusion technique in 0.2M DL-Malic acid pH 7.0, 20% PEG 3350 as reservoir solution. The protein was previously incubated with 3x molar excess of compound for 3h at 4C. Crystallization drops were prepared from 0.5ul of protein solution and 0.5ul of reservoir, and incubated for 10 days at 20C. Crystals were cryoprotected in 30% Glycerol and frozen in liquid nitrogen prior to data collection.

Crystal Properties
Matthews coefficient	Solvent content
2.65	53.54

Symmetry
Space Group	P 21 21 21

Diffraction Experiment
ID #	Crystal ID	Scattering Type	Data Collection Temperature	Detector	Detector Type	Details	Collection Date	Monochromator	Protocol
1	1	x-ray	100	PIXEL	DECTRIS PILATUS 2M		2018-01-31	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	ELETTRA BEAMLINE 5.2R	1.0	ELETTRA	5.2R

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	Rpim I (All)	CC (Half)	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	47.27	99.8	0.084	0.991	7.4	3.7		39567

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	Rpim I (All)	CC (Half)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1	2.3	2.38	100		0.72	0.57	1.5	3.8

Statistics
Diffraction ID	Structure Solution Method	Cross Validation method	Starting model	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	1Q5K	2.3	47.27	37543	1969	99.62	0.19483	0.19236	0.24047	RANDOM	37.707

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]
-1.1			1.14		-0.04

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	33.163
r_dihedral_angle_4_deg	20.277
r_dihedral_angle_3_deg	15.522
r_long_range_B_refined	7.996
r_long_range_B_other	7.993
r_dihedral_angle_1_deg	6.522
r_scangle_other	5.098
r_mcangle_it	4.549
r_mcangle_other	4.548
r_scbond_it	3.157

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	33.163
r_dihedral_angle_4_deg	20.277
r_dihedral_angle_3_deg	15.522
r_long_range_B_refined	7.996
r_long_range_B_other	7.993
r_dihedral_angle_1_deg	6.522
r_scangle_other	5.098
r_mcangle_it	4.549
r_mcangle_other	4.548
r_scbond_it	3.157
r_scbond_other	3.157
r_mcbond_it	2.807
r_mcbond_other	2.807
r_angle_refined_deg	1.386
r_angle_other_deg	0.994
r_chiral_restr	0.066
r_bond_refined_d	0.009
r_gen_planes_refined	0.006
r_bond_other_d	0.002
r_gen_planes_other	0.001
r_nbd_refined
r_nbd_other
r_nbtor_refined
r_nbtor_other
r_xyhbond_nbd_refined
r_xyhbond_nbd_other
r_metal_ion_refined
r_metal_ion_other
r_symmetry_vdw_refined
r_symmetry_vdw_other
r_symmetry_hbond_refined
r_symmetry_hbond_other
r_symmetry_metal_ion_refined
r_symmetry_metal_ion_other
r_scangle_it
r_rigid_bond_restr
r_sphericity_free
r_sphericity_bonded