Experiment: 3H20

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	VAPOR DIFFUSION, HANGING DROP	5.5	298	0.3M ammonium sulfate, 22% (wt/vol) PEG monomethyl ether 2000, 5% (vol/vol) gamma-butyrolactone, 100mM sodium acetate pH 5.5, VAPOR DIFFUSION, HANGING DROP, temperature 298K

Crystal Properties
Matthews coefficient	Solvent content
2.44	49.64

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 91.74	α = 90
b = 91.74	β = 90
c = 83.48	γ = 90

Symmetry
Space Group	P 43 21 2

Diffraction

Diffraction Experiment
ID #	Crystal ID	Scattering Type	Data Collection Temperature	Detector	Detector Type	Details	Collection Date	Monochromator	Protocol
1	1	x-ray	100	CCD	ADSC QUANTUM 4		2006-07-04	M	SINGLE WAVELENGTH
2	1	x-ray	100	CCD	ADSC QUANTUM 4		2005-11-26	M	MAD
3	1
4	1
1,2	1

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	ESRF BEAMLINE ID14-2	0.931	ESRF	ID14-2
2	SYNCHROTRON	ESRF BEAMLINE ID14-2	1.2557, 1.0442, 1.1406, 1.1402	ESRF	ID14-2

Data Collection

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	Net I Over Average Sigma (I)	Redundancy	Number Reflections (All)	Number Reflections (Observed)	Observed Criterion Sigma (F)	Observed Criterion Sigma (I)	B (Isotropic) From Wilson Plot
1,2	1.98	50	99.8			24819	24774	2	2

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1,2	1.985	2.036	100

Refinement

Statistics
Diffraction ID	Structure Solution Method	Cross Validation method	Resolution (High)	Resolution (Low)	Number Reflections (All)	Number Reflections (Observed)	Number Reflections (R-Free)	Percent Reflections (Observed)	R-Factor (All)	R-Factor (Observed)	R-Work	R-Free	R-Free Selection Details	Mean Isotropic B
X-RAY DIFFRACTION	MAD	THROUGHOUT	1.99	19.63	24819	24774	1026	100	0.197	0.197	0.195	0.232	RANDOM	36.055

Temperature Factor Modeling
Anisotropic B[1][1]	Anisotropic B[1][2]	Anisotropic B[1][3]	Anisotropic B[2][2]	Anisotropic B[2][3]	Anisotropic B[3][3]
-0.03			-0.03		0.06

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	35.762
r_dihedral_angle_4_deg	14.981
r_dihedral_angle_3_deg	13.886
r_dihedral_angle_1_deg	5.209
r_scangle_it	2.516
r_scbond_it	1.536
r_angle_refined_deg	1.096
r_mcangle_it	0.838
r_mcbond_it	0.536
r_nbtor_refined	0.282

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	35.762
r_dihedral_angle_4_deg	14.981
r_dihedral_angle_3_deg	13.886
r_dihedral_angle_1_deg	5.209
r_scangle_it	2.516
r_scbond_it	1.536
r_angle_refined_deg	1.096
r_mcangle_it	0.838
r_mcbond_it	0.536
r_nbtor_refined	0.282
r_nbd_refined	0.182
r_symmetry_vdw_refined	0.169
r_xyhbond_nbd_refined	0.13
r_symmetry_hbond_refined	0.099
r_chiral_restr	0.072
r_bond_refined_d	0.01
r_gen_planes_refined	0.003

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	2164
Nucleic Acid Atoms
Solvent Atoms	253
Heterogen Atoms	24

Software

Software
Software Name	Purpose
XSCALE	data scaling
REFMAC	refinement
PDB_EXTRACT	data extraction
ADSC	data collection
XDS	data reduction
SHELX	phasing

RCSB PDB Core Operations are funded by the U.S. National Science Foundation (DBI-2321666), the US Department of Energy (DE-SC0019749), and the National Cancer Institute, National Institute of Allergy and Infectious Diseases, and National Institute of General Medical Sciences of the National Institutes of Health under grant R01GM133198.