Experiment: 4RWB

X-RAY DIFFRACTION

Crystallization

Crystalization Experiments
ID	Method	pH	Temperature	Details
1	monoolein lipidic cubic phase	6.5	298	Peptide combined with monoolein at 15-20% (w/w) by codissolving in trifluoroethanol, LCP generated by mixing vacuum-dried solid components with water at 60:40 lipid:water ratio. 200 nL LCP bolus combined with 1 uL solution containing 0.1 M ADA pH 6.5, 24% MPD in glass sandwich plates. Crystals grew in less than 1 day. , monoolein lipidic cubic phase, temperature 298K

Crystal Properties
Matthews coefficient	Solvent content
2.36	47.99

Crystal Data

Unit Cell
Length ( Å )	Angle ( ˚ )
a = 40.93	α = 90
b = 41.23	β = 95.68
c = 27.93	γ = 90

Symmetry
Space Group	P 1 21/c 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	CCD	MARMOSAIC 225 mm CCD		2012-06-14	M	SINGLE WAVELENGTH

Radiation Source
ID #	Source	Type	Wavelength List	Synchrotron Site	Beamline
1	SYNCHROTRON	APS BEAMLINE 21-ID-F	0.97872	APS	21-ID-F

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	19.39	96.2	0.127	8.88	7.14		6119			17.3

Highest Resolution Shell
ID #	Resolution (High)	Resolution (Low)	Percent Possible (All)	Percent Possible (Observed)	R-Sym I (Observed)	Mean I Over Sigma (Observed)	Redundancy	Number Unique Reflections (All)
1	2	2.03	95.9		0.56	2.27	7.2

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	PDB entry 3LBW	2	19.39	5919	283	96.64	0.2816	0.2808	0.2956	RANDOM	28.352

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]
2.77		-0.32	-2.71		-0.03

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	33.808
r_dihedral_angle_4_deg	19.944
r_dihedral_angle_3_deg	10.465
r_dihedral_angle_1_deg	3.616
r_angle_refined_deg	1.641
r_angle_other_deg	0.799
r_chiral_restr	0.086
r_bond_refined_d	0.013
r_gen_planes_refined	0.007
r_bond_other_d	0.001

RMS Deviations
Key	Refinement Restraint Deviation
r_dihedral_angle_2_deg	33.808
r_dihedral_angle_4_deg	19.944
r_dihedral_angle_3_deg	10.465
r_dihedral_angle_1_deg	3.616
r_angle_refined_deg	1.641
r_angle_other_deg	0.799
r_chiral_restr	0.086
r_bond_refined_d	0.013
r_gen_planes_refined	0.007
r_bond_other_d	0.001
r_gen_planes_other	0.001

Non-Hydrogen Atoms Used in Refinement
Non-Hydrogen Atoms	Number
Protein Atoms	354
Nucleic Acid Atoms
Solvent Atoms	4
Heterogen Atoms	75

Software

Software
Software Name	Purpose
XPREP	data reduction
REFMAC	refinement
PDB_EXTRACT	data extraction
EMBL	data collection
XDS	data reduction
XSCALE	data scaling
PHASER	phasing

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.