5T8E

Synthesis and biological evaluation of novel selective androgen receptor modulators (SARMs). Part II: Optimization of 4-(pyrrolidin-1-yl)benzonitrile derivatives

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ALS BEAMLINE 5.0.2
Synchrotron site	ALS
Beamline	5.0.2
Temperature [K]	80
Detector technology	CCD
Collection date	2006-07-22
Detector	ADSC QUANTUM 315r
Wavelength(s)	1.0
Spacegroup name	P 21 21 21
Unit cell lengths	53.804, 66.195, 70.932
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	35.980 - 2.710
R-factor	0.1757
Rwork	0.173
R-free	0.23810
RMSD bond length	0.007
RMSD bond angle	1.003
Data reduction software	HKL-2000
Data scaling software	SCALEPACK
Phasing software	MOLREP
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	35.980	50.000	2.800
High resolution limit [Å]	2.700	5.810	2.700
Rmerge	0.077	0.060	0.234
Total number of observations	46881
Number of reflections	6954
<I/σ(I)>	16.9
Completeness [%]	95.6	99	81.6
Redundancy	6.7	6.8	5.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7.2	293	Protein Storage Buffer: 25mM HEPES pH 7.2, 150mM LiSO4, 10mM DTT, 10% Glycerol, 0.1% bOG, 100uM inhibitor Crystallization Buffer: ~1M ammonium phosphate dibasic