3OCS

Crystal structure of bruton's tyrosine kinase in complex with inhibitor CGI1746


X-RAY DIFFRACTION

Starting Model(s)

Initial Refinement Model(s)
TypeSourceAccession CodeDetails
experimental modelPDB 1K2P 

Crystallization

Crystalization Experiments
IDMethodpHTemperatureDetails
1VAPOR DIFFUSION, SITTING DROP728914% PEG 10,000, 150 MM LI2SO4, 100 MM IMIDAZOLE, PH 7.0, 0.75% OCTYL-B-D-GLUCOPYRANOSIDE, VAPOR DIFFUSION, TEMPERATURE 289K, VAPOR DIFFUSION, SITTING DROP
Crystal Properties
Matthews coefficientSolvent content
2.2545.22

Crystal Data

Unit Cell
Length ( Å )Angle ( ˚ )
a = 108.386α = 90
b = 108.386β = 90
c = 41.974γ = 120
Symmetry
Space GroupP 61

Diffraction

Diffraction Experiment
ID #Crystal IDScattering TypeData Collection TemperatureDetectorDetector TypeDetailsCollection DateMonochromatorProtocol
11x-ray100CCDADSC QUANTUM 3152006-02-01MSINGLE WAVELENGTH
Radiation Source
ID #SourceTypeWavelength ListSynchrotron SiteBeamline
1SYNCHROTRONSSRL BEAMLINE BL1-50.97944SSRLBL1-5

Data Collection

Overall
ID #Resolution (High)Resolution (Low)Percent Possible (Observed)R Merge 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
11.894.07990.0729.14.726112
Highest Resolution Shell
ID #Resolution (High)Resolution (Low)Percent Possible (All)Percent Possible (Observed)R Merge I (Observed)Mean I Over Sigma (Observed)RedundancyNumber Unique Reflections (All)
1.81.8691.10.5012.9

Refinement

Statistics
Diffraction IDStructure Solution MethodCross Validation methodStarting modelResolution (High)Resolution (Low)Number Reflections (Observed)Number Reflections (R-Free)Percent Reflections (Observed)R-Factor (Observed)R-WorkR-FreeR-Free Selection DetailsMean Isotropic B
X-RAY DIFFRACTIONMOLECULAR REPLACEMENTTHROUGHOUT1K2P1.894.072607913230.1840.1830.213RANDOM20.75
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]
0.520.260.52-0.78
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg29.729
r_dihedral_angle_4_deg19.782
r_dihedral_angle_3_deg14.245
r_dihedral_angle_1_deg10.621
r_scangle_it3.495
r_scbond_it2.368
r_angle_refined_deg1.494
r_mcangle_it1.426
r_mcbond_it0.965
r_nbtor_refined0.312
RMS Deviations
KeyRefinement Restraint Deviation
r_dihedral_angle_2_deg29.729
r_dihedral_angle_4_deg19.782
r_dihedral_angle_3_deg14.245
r_dihedral_angle_1_deg10.621
r_scangle_it3.495
r_scbond_it2.368
r_angle_refined_deg1.494
r_mcangle_it1.426
r_mcbond_it0.965
r_nbtor_refined0.312
r_symmetry_hbond_refined0.218
r_nbd_refined0.201
r_symmetry_vdw_refined0.197
r_xyhbond_nbd_refined0.142
r_chiral_restr0.114
r_bond_refined_d0.014
r_gen_planes_refined0.007
Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen AtomsNumber
Protein Atoms2100
Nucleic Acid Atoms
Solvent Atoms159
Heterogen Atoms62

Software

Software
Software NamePurpose
MOLREPphasing
REFMACrefinement
HKL-2000data reduction
HKL-2000data scaling