4Q1E

Human dCK C4S-S74E mutant in complex with UDP and the inhibitor 10 {2-{[(1R/S)-1-{2-[3-(2-fluoroethoxy)-4-methoxyphenyl]-5-methyl-1,3-thiazol 4-yl}ethyl]sulfanyl}pyrimidine-4,6-diamine}


X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, HANGING DROP7.52851.5 M trisodium citrate dehydrate and 25 mM HEPES pH 7.5, VAPOR DIFFUSION, HANGING DROP, temperature 285K
Crystal Properties
Matthews coefficientSolvent content
2.2144.27

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 68.736α = 90
b = 68.736β = 90
c = 122.206γ = 90
Symmetry
Space GroupP 41

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray93IMAGE PLATERIGAKU RAXIS IV++2013-05-28MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1ROTATING ANODERIGAKU RU2001.5418

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Sym I (Observed)Net I Over Average Sigma (I)RedundancyNumber Reflections (All)Number Reflections (Observed)Observed Criterion Sigma (F)Observed Criterion Sigma (I)B (Isotropic) From Wilson Plot
11.853096.90.02821.624676246762
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R-Sym I (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
11.851.9682.80.4041.996415

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodStarting modelResolution (High)Resolution (Low)Number Reflections (All)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-Factor (All)R-Factor (Observed)R-WorkR-FreeR-Free Selection DetailsMean Isotropic B
X-RAY DIFFRACTIONMOLECULAR REPLACEMENTTHROUGHOUTPDB entry 4JLN1.8527.924374743747227395.370.176090.176090.173990.21765RANDOM38.281
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]
-6.71-6.7113.43
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg41.675
r_dihedral_angle_4_deg18.363
r_dihedral_angle_3_deg16.7
r_dihedral_angle_1_deg6.131
r_long_range_B_refined5.4
r_long_range_B_other5.352
r_scangle_other3.54
r_mcangle_it3.4
r_mcangle_other3.4
r_mcbond_it2.497
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg41.675
r_dihedral_angle_4_deg18.363
r_dihedral_angle_3_deg16.7
r_dihedral_angle_1_deg6.131
r_long_range_B_refined5.4
r_long_range_B_other5.352
r_scangle_other3.54
r_mcangle_it3.4
r_mcangle_other3.4
r_mcbond_it2.497
r_mcbond_other2.491
r_scbond_it2.473
r_scbond_other2.473
r_angle_refined_deg1.673
r_angle_other_deg0.961
r_chiral_restr0.085
r_bond_refined_d0.013
r_gen_planes_refined0.006
r_bond_other_d0.003
r_gen_planes_other0.001
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms3785
Nucleic Acid Atoms
Solvent Atoms185
Heterogen Atoms166

Software

Software
Software NamePurpose
CrystalCleardata collection
MOLREPphasing
REFMACrefinement
XDSdata reduction
XDSdata scaling