Experiment: 3ECD

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	VAPOR DIFFUSION, SITTING DROP	7	289	PACT SCREEN CONDITION C6, 20% PEG 6000, 0.2 M NaCl, 0.1 M HEPES-KOH pH 7.0, 24.1 mg/mL protein, 0.4/0.4 uL drops, Crystal ID 109933C6, VAPOR DIFFUSION, SITTING DROP, temperature 289K

Crystal Properties
Matthews coefficient	Solvent content
2.16	42.95

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 58.212	α = 97.79
b = 61.865	β = 89.97
c = 117.577	γ = 110.24

Symmetry
Space Group	P 1

Diffraction

Diffraction Experiment
ID #	Crystal ID	Scattering Type	Data Collection Temperature	Detector	Detector Type	Details	Collection Date	Monochromator	Protocol
1	1	x-ray	100				2008-08-23	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	ALS BEAMLINE 5.0.2	0.99994	ALS	5.0.2

Data Collection

Overall
ID #	Resolution (High)	Resolution (Low)	Percent Possible (Observed)	R Merge I (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	1.4	58.222	94.6	0.044	0.044	12.358	2.1	408650	190206

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	R Merge I (Observed)	R-Sym I (Observed)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1	1.6	1.69	86.4		0.408	0.408	1.8	2.1	25383

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	1KKJ	1.6	58.222	190195	9593	94.61	0.188	0.187	0.206	RANDOM	20.891

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]
-0.29	0.52	-0.09	1.13	0.24	-0.41

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	32.731
r_dihedral_angle_4_deg	14.934
r_dihedral_angle_3_deg	13.699
r_dihedral_angle_1_deg	5.452
r_scangle_it	2.595
r_scbond_it	1.472
r_angle_other_deg	1.33
r_angle_refined_deg	1.2
r_mcangle_it	0.911
r_mcbond_it	0.476

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	32.731
r_dihedral_angle_4_deg	14.934
r_dihedral_angle_3_deg	13.699
r_dihedral_angle_1_deg	5.452
r_scangle_it	2.595
r_scbond_it	1.472
r_angle_other_deg	1.33
r_angle_refined_deg	1.2
r_mcangle_it	0.911
r_mcbond_it	0.476
r_mcbond_other	0.086
r_chiral_restr	0.058
r_bond_refined_d	0.008
r_gen_planes_refined	0.005
r_gen_planes_other	0.002
r_bond_other_d	0.001

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	11605
Nucleic Acid Atoms
Solvent Atoms	1607
Heterogen Atoms	24

Software

Software
Software Name	Purpose
MOSFLM	data reduction
SCALA	data scaling
MOLREP	phasing
REFMAC	refinement
PDB_EXTRACT	data extraction

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.