6SUS

Crystal structure of RTX domain blocks IV and V of adenylate cyclase toxin from Bordetella pertussis

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	VAPOR DIFFUSION, HANGING DROP		291	0.2 M NH4NO3 20% w/v PEG 3350

Crystal Properties
Matthews coefficient	Solvent content
4.14	70.27

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 91.771	α = 90
b = 91.771	β = 90
c = 104.465	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	90	CCD	RAYONIX MX-225		2014-03-26	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	BESSY BEAMLINE 14.2	0.918	BESSY	14.2

Data Collection

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	R Merge I (Observed)	Rrim I (All)	CC (Half)	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	1.76	50	99.8	0.052	0.055	1	24.66	8.94		44820

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	R Merge I (Observed)	Rrim I (All)	CC (Half)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1	1.76	1.87	99.5		0.831	0.881	0.858	2.69

Refinement

Statistics
Diffraction ID	Structure Solution Method	Cross Validation method	Starting model	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	MOLECULAR REPLACEMENT	THROUGHOUT	5CVW	1.76	45.89	42719	2100	99.84	0.1844	0.1836	0.2008	RANDOM	35.519

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]
-0.02			-0.02		0.04

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	36.939
r_dihedral_angle_4_deg	14.261
r_dihedral_angle_3_deg	12.575
r_dihedral_angle_1_deg	6.927
r_angle_other_deg	3.978
r_mcangle_it	3.213
r_mcbond_it	2.283
r_mcbond_other	2.282
r_angle_refined_deg	1.187
r_chiral_restr	0.053

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	36.939
r_dihedral_angle_4_deg	14.261
r_dihedral_angle_3_deg	12.575
r_dihedral_angle_1_deg	6.927
r_angle_other_deg	3.978
r_mcangle_it	3.213
r_mcbond_it	2.283
r_mcbond_other	2.282
r_angle_refined_deg	1.187
r_chiral_restr	0.053
r_bond_refined_d	0.008
r_gen_planes_refined	0.006
r_gen_planes_other	0.006
r_bond_other_d	0.001

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	1871
Nucleic Acid Atoms
Solvent Atoms	177
Heterogen Atoms	63

Software

Software
Software Name	Purpose
REFMAC	refinement
XDS	data reduction
XDS	data scaling
PHASER	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.