1NQ9

Crystal Structure of Antithrombin in the Pentasaccharide-Bound Intermediate State

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SRS BEAMLINE PX14.1
Synchrotron site	SRS
Beamline	PX14.1
Temperature [K]	100
Detector technology	CCD
Collection date	2002-11-30
Detector	ADSC QUANTUM 4
Wavelength(s)	1.4880
Spacegroup name	P 1 21 1
Unit cell lengths	69.679, 86.760, 96.921
Unit cell angles	90.00, 109.54, 90.00

Refinement procedure

Resolution	24.430 - 2.600
Rwork	0.209
R-free	0.25000
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1e05
RMSD bond length	0.008
RMSD bond angle	1.300
Data scaling software	SCALA
Phasing software	MOLREP
Refinement software	CNS (1.0)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	24.620	2.740
High resolution limit [Å]	2.600	2.600
Rmerge	0.092	0.571 *
Total number of observations	120627 *
Number of reflections	33466 *	4740 *
<I/σ(I)>	6.9	1.9
Completeness [%]	99.6 *	99.6 *
Redundancy	3.6	3.1

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.4	292	PEG 3350, Ammonium Fluoride, Tris, glycerol, 1,8-ANS , pH 7.4, VAPOR DIFFUSION, HANGING DROP, temperature 292K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	antithrombin	7.2 (mg/ml)
2	1	reservoir	Tris	10 (mM)	pH7.4
3	1	reservoir		128 (mM)
4	1	reservoir	PEG3350	12.8 (%)
5	1	reservoir	glycerol	20 (%)
6	1	reservoir	ANS	0.35 (mg/ml)