1B4D

AMIDOCARBAMATE INHIBITOR OF GLYCOGEN PHOSPHORYLASE

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	EMBL/DESY, HAMBURG BEAMLINE X11
Synchrotron site	EMBL/DESY, HAMBURG
Beamline	X11
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	1995-10-18
Detector	MAR scanner 180 mm plate
Spacegroup name	P 43 21 2
Unit cell lengths	126.680, 126.680, 115.350
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	20.000 - 2.000
R-factor	0.182
Rwork	0.182
R-free	0.22900
Structure solution method	OTHER
Starting model (for MR)	1a8i
RMSD bond length	0.008
RMSD bond angle	23.400 *
Data reduction software	DENZO
Data scaling software	SCALEPACK
Phasing software	CCP4
Refinement software	X-PLOR (3.8)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	20.000	2.070
High resolution limit [Å]	2.000	2.000
Rmerge	0.060	0.219
Number of reflections	62995
<I/σ(I)>	15.67	6.2
Completeness [%]	99.4	99.6
Redundancy	6.6

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	unknown *	6.7	289	CO-CRYSTALLIZED COMPLEX WAS OBTAINED FROM 0.01 M BES, PH 6.7, 0.003 M DTT, 0.001 M SPERMINE, 0.0001 M SODIUM EDTA, 0.02 % SODIUM AZIDE AND 0.01 M AMIDOCARBAMATE AT 16 DEGREES C. JUST BEFORE DATA COLLECTION, THE CRYSTALS WERE TRANSFERRED TO A FRESH SOLUTION OF THE ABOVE BUFFER CONTAINING 30% GLYCEROL FOR 30-60 SEC., temperature 289K