3R4N

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	2006-02-26
Detector	MAR scanner 345 mm plate
Wavelength(s)	1.5418
Spacegroup name	P 21 21 21
Unit cell lengths	45.875, 79.404, 118.506
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	17.740 - 2.000
R-factor	0.188
Rwork	0.186
R-free	0.22000
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.005
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]	17.740	2.070
High resolution limit [Å]	2.000	2.000
Rmerge	0.059	0.229
Number of reflections	29344
<I/σ(I)>	24.5	6.95
Completeness [%]	99.4	98.4
Redundancy	4.2	4

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	4.5	286	20 % Ethylene glycol, 0.1 M citrate phosphate, 20 mM TCEP, pH 4.5, VAPOR DIFFUSION, HANGING DROP, temperature 286K