1BKX

A BINARY COMPLEX OF THE CATALYTIC SUBUNIT OF CAMP-DEPENDENT PROTEIN KINASE AND ADENOSINE FURTHER DEFINES CONFORMATIONAL FLEXIBILITY

Experimental procedure

Source type	ROTATING ANODE
Source details	RIGAKU RUH2R
Temperature [K]	277
Detector technology	AREA DETECTOR
Collection date	1994-09-13
Detector	XUONG-HAMLIN MULTIWIRE
Spacegroup name	P 21 21 21
Unit cell lengths	55.850, 73.230, 98.720
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	10.000 - 2.600
R-factor	0.219
Rwork	0.205
R-free	0.34000
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1ctp
RMSD bond length	0.020
RMSD bond angle	20.200 *
Data reduction software	UCSD
Data scaling software	UCSD
Phasing software	X-PLOR
Refinement software	TNT (5E)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	30.000	2.700
High resolution limit [Å]	2.600	2.600
Rmerge	0.094 *
Number of reflections	10720
<I/σ(I)>	8.5	1
Completeness [%]	86.0	74
Redundancy	2.5	1.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	8	4 *	THE RC.ADE BINARY COMPLEX CRYSTALS WERE GROWN AT 4 C BY THE HANGING-DROP VAPOR DIFFUSION METHOD. THE CRYSTALLIZATION DROPLET CONTAINED PROTEIN (0.5 MM), ADENOSINE (3 MM) AND 2-METHYL-2,4-PENTANEDIOL (MPD; 4%) IN 100 MM BICINE BUFFER AT PH 8.0. THE CRYSTALLIZATION WELL SOLUTION WAS MADE UP OF 15% MPD AND 100 MM AMMONIUM-SULFATE IN BICINE BUFFER (100 MM; PH 8.0). THE CRYSTALS GREW OVER THE COURSE OF 8-12 WEEKS TO A FINAL SIZE OF 0.2 X 0.3 X 0.5 MM3., vapor diffusion - hanging drop, temperature 277K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	protein	0.5 (mM)
2	1	drop	adenosine	3 (mM)
3	1	drop	MPD	4 (%)
4	1	drop	bicine	100 (mM)
5	1	reservoir	MPD	15 (%)
6	1	reservoir	ammonium sulfate	100 (mM)
7	1	reservoir	bicine	100 (mM)