3R4M
Optimization of Potent, Selective, and Orally Bioavailable Pyrrolodinopyrimidine-containing Inhibitors of Heat Shock Protein 90. Identification of Development Candidate 2-amino-4-{4-chloro-2-[2-(4-fluoro-1H-pyrazol-1-yl)ethoxy]-6-methylphenyl}-N-(2,2-difluoropropyl)-5,7-dihydro-6H-pyrrolo[3,4-d]pyrimidine-6-carboxamide
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | ROTATING ANODE |
Source details | ENRAF-NONIUS FR591 |
Temperature [K] | 98 |
Detector technology | IMAGE PLATE |
Collection date | 2004-04-30 |
Detector | MAR scanner 345 mm plate |
Wavelength(s) | 1.5418 |
Spacegroup name | P 1 21 1 |
Unit cell lengths | 54.196, 44.126, 53.263 |
Unit cell angles | 90.00, 115.65, 90.00 |
Refinement procedure
Resolution | 24.400 - 1.700 |
R-factor | 0.196 |
Rwork | 0.194 |
R-free | 0.22300 |
Structure solution method | MOLECULAR REPLACEMENT |
RMSD bond length | 0.004 |
RMSD bond angle | 0.800 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Phasing software | CNX |
Refinement software | CNX |
Data quality characteristics
Overall | Outer shell | |
Low resolution limit [Å] | 24.400 | 1.760 |
High resolution limit [Å] | 1.700 | 1.700 |
Rmerge | 0.047 | 0.083 |
Number of reflections | 20874 | |
<I/σ(I)> | 27.2 | 13.4 |
Completeness [%] | 83.7 | 93.4 |
Redundancy | 3.6 | 3.2 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 5.2 | 286 | 30 % PEG MME 550, 0.1 M CaCl2, 0.1 M cacodylate, pH 5.2, VAPOR DIFFUSION, HANGING DROP, temperature 286K |