3V6I

Crystal structure of the peripheral stalk of Thermus thermophilus H+-ATPase/synthase at 2.25 A resolution

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	VAPOR DIFFUSION, HANGING DROP	7.5	293	100mM HEPES (pH 7.5), 200mM Calcium acetate, 40% (v/v) PEG 400, VAPOR DIFFUSION, HANGING DROP, temperature 293K

Crystal Properties
Matthews coefficient	Solvent content
3.06	59.78

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 102.51	α = 90
b = 208.69	β = 90
c = 36.9	γ = 90

Symmetry
Space Group	P 21 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 315r		2006-09-03	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	ESRF BEAMLINE ID14-4	0.9393	ESRF	ID14-4

Data Collection

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	R Sym I (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	2.24	19.67	97.2	0.057	10.7	2.5	37768	37768

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	R Merge I (Observed)	R-Sym I (Observed)	Rrim I (All)	Rpim I (All)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1	2.25	2.37	98.7		0.533	0.533	0.669	0.396	1.4	2.5	5533

Refinement

Statistics
Diffraction ID	Structure Solution Method	Cross Validation method	Resolution (High)	Resolution (Low)	Number Reflections (Observed)	Number Reflections (R-Free)	Percent Reflections (Observed)	R-Factor (Observed)	R-Work	R-Free	R-Free Selection Details	Mean Isotropic B
X-RAY DIFFRACTION	MIRAS	THROUGHOUT	2.25	19.67	32182	1685	87.33	0.2252	0.2232	0.2629	RANDOM	13.0229

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]
1.92			-3.04		1.12

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	28.247
r_dihedral_angle_4_deg	16.618
r_dihedral_angle_3_deg	14.915
r_scangle_it	8.772
r_scbond_it	5.216
r_dihedral_angle_1_deg	4.606
r_mcangle_it	3.229
r_rigid_bond_restr	2.472
r_mcbond_it	1.772
r_angle_refined_deg	1.224

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	28.247
r_dihedral_angle_4_deg	16.618
r_dihedral_angle_3_deg	14.915
r_scangle_it	8.772
r_scbond_it	5.216
r_dihedral_angle_1_deg	4.606
r_mcangle_it	3.229
r_rigid_bond_restr	2.472
r_mcbond_it	1.772
r_angle_refined_deg	1.224
r_chiral_restr	0.081
r_bond_refined_d	0.01
r_gen_planes_refined	0.008

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	4015
Nucleic Acid Atoms
Solvent Atoms	94
Heterogen Atoms	8

Software

Software
Software Name	Purpose
SCALA	data scaling
SHARP	phasing
SOLOMON	phasing
REFMAC	refinement
PDB_EXTRACT	data extraction
XDS	data reduction

RCSB PDB Core Operations are funded by the National Science Foundation (DBI-1832184), 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.