3R4O
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 | RIGAKU |
| Temperature [K] | 98 |
| Detector technology | IMAGE PLATE |
| Collection date | 2007-04-15 |
| Detector | MAR scanner 345 mm plate |
| Wavelength(s) | 1.5418 |
| Spacegroup name | P 21 21 21 |
| Unit cell lengths | 43.149, 79.523, 130.101 |
| Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
| Resolution | 19.880 - 2.650 |
| R-factor | 0.215 |
| Rwork | 0.211 |
| R-free | 0.28500 |
| Structure solution method | MOLECULAR REPLACEMENT |
| RMSD bond length | 0.006 |
| RMSD bond angle | 0.900 |
| Data reduction software | HKL-2000 |
| Data scaling software | SCALEPACK |
| Phasing software | CNX |
| Refinement software | CNX |
Data quality characteristics
| Overall | Outer shell | |
| Low resolution limit [Å] | 19.880 | 2.740 |
| High resolution limit [Å] | 2.650 | 2.650 |
| Rmerge | 0.074 | 0.211 |
| Number of reflections | 11758 | |
| <I/σ(I)> | 18.4 | 6.45 |
| Completeness [%] | 86.2 | 79.6 |
| Redundancy | 4.7 | 4.3 |
Crystallization Conditions
| crystal ID | method | pH | temperature | details |
| 1 | VAPOR DIFFUSION, HANGING DROP | 4.5 | 286 | 5 % Ethylene glycol, 0.1 M phosphate-citrate, pH 4.5, 20 mM TCEP, VAPOR DIFFUSION, HANGING DROP, temperature 286K |
