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