3R91

Macrocyclic lactams as potent Hsp90 inhibitors with excellent tumor exposure and extended biomarker activity.

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU FR-E+ SUPERBRIGHT
Temperature [K]	93
Detector technology	CCD
Collection date	2008-05-29
Detector	RIGAKU SATURN 92
Wavelength(s)	1.5418
Spacegroup name	I 2 2 2
Unit cell lengths	67.042, 90.250, 97.797
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	27.648 - 1.579
R-factor	0.1869
Rwork	0.186
R-free	0.19880
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	3bm9
RMSD bond length	0.006
RMSD bond angle	1.009
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER
Refinement software	PHENIX ((phenix.refine))

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	27.650	1.620
High resolution limit [Å]	1.579	1.579
Number of reflections	30881
<I/σ(I)>	27.4	1.35
Completeness [%]	75.2	44
Redundancy	7.5	1.3

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.5	277	22% PEG3350, 0.175 M MAGNESIUM NITRATE, pH 7.5, TEMPERATURE 277K; FROZEN BY 1-STEP TRANSFER TO 25% GLYCEROL, 17% PEG3350, 0.13M MAGNESIUM NITRATE, VAPOR DIFFUSION, HANGING DROP