5HBE

CDK8-CYCC IN COMPLEX WITH 8-[3-Chloro-5-(1-methyl-2,2-dioxo-2, 3-dihydro-1H-2l6-benzo[c]isothiazol-5-yl)-pyridin- 4-yl]-1-oxa-3,8-diaza-spiro[4.5]decan-2-one

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	VAPOR DIFFUSION, HANGING DROP	6.9	293	RESERVOIR SOLUTION : pH 6.90

Crystal Properties
Matthews coefficient	Solvent content
3.09	60.27

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 71.007	α = 90
b = 71.115	β = 90
c = 173.152	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	100	PIXEL	PSI PILATUS 6M		2012-07-01	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	SLS BEAMLINE X06SA	1.00000	SLS	X06SA

Data Collection

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	R Merge I (Observed)	Rrim I (All)	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	2.38	86.58	99.2	0.06	0.068	18.73	4.6		35972			54.225

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	R Merge I (Observed)	Rrim I (All)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1	2.38	2.63	99.6		0.516	0.018	3.36	4.8

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	2.38	86.58	34516	1180	99.23	0.2296	0.2287	0.2555	RANDOM	37.069

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]
-4.19			-2.06		6.26

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	33.917
r_dihedral_angle_4_deg	16.325
r_dihedral_angle_3_deg	12.956
r_dihedral_angle_1_deg	5.617
r_scangle_it	5.201
r_scbond_it	3.453
r_mcangle_it	2.395
r_mcbond_it	1.354
r_angle_refined_deg	1.155
r_angle_other_deg	0.987

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	33.917
r_dihedral_angle_4_deg	16.325
r_dihedral_angle_3_deg	12.956
r_dihedral_angle_1_deg	5.617
r_scangle_it	5.201
r_scbond_it	3.453
r_mcangle_it	2.395
r_mcbond_it	1.354
r_angle_refined_deg	1.155
r_angle_other_deg	0.987
r_mcbond_other	0.285
r_chiral_restr	0.067
r_bond_refined_d	0.009
r_gen_planes_refined	0.004
r_bond_other_d	0.001
r_gen_planes_other	0.001

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	5055
Nucleic Acid Atoms
Solvent Atoms	55
Heterogen Atoms	50

Software

Software
Software Name	Purpose
XSCALE	data scaling
REFMAC	refinement
PDB_EXTRACT	data extraction
XDS	data reduction

RCSB PDB Core Operations are funded by the U.S. National Science Foundation (DBI-2321666), 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 R01GM157729.