PDB-6hsv: Engineered higher-order assembly of Cholera Toxin B subunits via ...

Basic information

• Entry: Database: PDB / ID: 6hsv
• Title: Engineered higher-order assembly of Cholera Toxin B subunits via the addition of C-terminal parallel coiled-coiled domains
• Components: Toxin B subunit
• Keywords: TOXIN / Cholera toxin B / CTB / parallel coiled coils / higher order assembly / self assembly / designed protein / nanotube

Function / homology

Function:

host cell surface binding / galactose binding / catalytic complex / : / positive regulation of tyrosine phosphorylation of STAT protein / toxin activity / periplasmic space / host cell plasma membrane / extracellular region / membrane

Domain/homology:

Heat-labile enterotoxin, B chain / Heat-labile enterotoxin beta chain / OB fold (Dihydrolipoamide Acetyltransferase, E2P) - #110 / Enterotoxin / OB fold (Dihydrolipoamide Acetyltransferase, E2P) / Beta Barrel / Mainly Beta

Component:

PHOSPHATE ION / Cholera enterotoxin subunit B / Toxin B subunit

• Biological species: Vibrio cholerae (bacteria)
• Method: X-RAY DIFFRACTION / SYNCHROTRON / MOLECULAR REPLACEMENT / Resolution: 2.45 Å
• Authors: Pearson, A.R. / Turnbull, W.B. / Ross, J.F. / Trinh, C.H. / Webb, M.E.

Funding support

United Kingdom, Germany, 7items

Organization	Grant number	Country
Wellcome Trust	089308/Z/09/Z	United Kingdom
Wellcome Trust	102572/B/13/Z	United Kingdom
Wellcome Trust	090932/Z/09/Z	United Kingdom
Wellcome Trust	094232/Z/10/Z	United Kingdom
Wellcome Trust	108466/Z/15/Z	United Kingdom
Biotechnology and Biological Sciences Research Council	BB/M005666/1	United Kingdom
German Research Foundation	EXC1074	Germany

• Citation: Journal: J.Am.Chem.Soc. / Year: 2019; Title: Directed Assembly of Homopentameric Cholera Toxin B-Subunit Proteins into Higher-Order Structures Using Coiled-Coil Appendages.; Authors: Ross, J.F. / Wildsmith, G.C. / Johnson, M. / Hurdiss, D.L. / Hollingsworth, K. / Thompson, R.F. / Mosayebi, M. / Trinh, C.H. / Paci, E. / Pearson, A.R. / Webb, M.E. / Turnbull, W.B.

History

Deposition	Oct 1, 2018	Deposition site: PDBE / Processing site: PDBE
Revision 1.0	Mar 20, 2019	Provider: repository / Type: Initial release
Revision 1.1	Apr 10, 2019	Group: Data collection / Database references / Category: citation / citation_author / pdbx_database_proc Item: _citation.journal_volume / _citation.page_first / _citation.page_last / _citation.title / _citation_author.identifier_ORCID / _citation_author.name
Revision 1.2	May 8, 2019	Group: Advisory / Data collection / Derived calculations Category: diffrn_source / pdbx_validate_close_contact / struct_conn / struct_conn_type Item: _diffrn_source.pdbx_synchrotron_site
Revision 1.3	Jul 10, 2019	Group: Data collection / Category: diffrn_source / Item: _diffrn_source.pdbx_synchrotron_site
Revision 1.4	Jan 24, 2024	Group: Data collection / Database references / Refinement description Category: chem_comp_atom / chem_comp_bond / database_2 / pdbx_initial_refinement_model / struct_ncs_dom_lim Item: _database_2.pdbx_DOI / _database_2.pdbx_database_accession / _struct_ncs_dom_lim.beg_auth_comp_id / _struct_ncs_dom_lim.beg_label_asym_id / _struct_ncs_dom_lim.beg_label_comp_id / _struct_ncs_dom_lim.beg_label_seq_id / _struct_ncs_dom_lim.end_auth_comp_id / _struct_ncs_dom_lim.end_label_asym_id / _struct_ncs_dom_lim.end_label_comp_id / _struct_ncs_dom_lim.end_label_seq_id

Assembly

Deposited unit

A: Toxin B subunit

B: Toxin B subunit

C: Toxin B subunit

D: Toxin B subunit

E: Toxin B subunit

F: Toxin B subunit

G: Toxin B subunit

H: Toxin B subunit

I: Toxin B subunit

J: Toxin B subunit

K: Toxin B subunit

L: Toxin B subunit

M: Toxin B subunit

N: Toxin B subunit

O: Toxin B subunit

P: Toxin B subunit

Q: Toxin B subunit

R: Toxin B subunit

S: Toxin B subunit

T: Toxin B subunit

hetero molecules

Summary:

• 281 kDa, 20 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	281,394	54
Polymers	277,598	20
Non-polymers	3,796	34
Water	10,521	584

1

A: Toxin B subunit

B: Toxin B subunit

C: Toxin B subunit

D: Toxin B subunit

E: Toxin B subunit

F: Toxin B subunit

G: Toxin B subunit

H: Toxin B subunit

I: Toxin B subunit

J: Toxin B subunit

K: Toxin B subunit

L: Toxin B subunit

M: Toxin B subunit

N: Toxin B subunit

O: Toxin B subunit

P: Toxin B subunit

Q: Toxin B subunit

R: Toxin B subunit

S: Toxin B subunit

T: Toxin B subunit

hetero molecules

A: Toxin B subunit

B: Toxin B subunit

C: Toxin B subunit

D: Toxin B subunit

E: Toxin B subunit

F: Toxin B subunit

G: Toxin B subunit

H: Toxin B subunit

I: Toxin B subunit

J: Toxin B subunit

K: Toxin B subunit

L: Toxin B subunit

M: Toxin B subunit

N: Toxin B subunit

O: Toxin B subunit

P: Toxin B subunit

Q: Toxin B subunit

R: Toxin B subunit

S: Toxin B subunit

T: Toxin B subunit

hetero molecules

A: Toxin B subunit

B: Toxin B subunit

C: Toxin B subunit

D: Toxin B subunit

E: Toxin B subunit

F: Toxin B subunit

G: Toxin B subunit

H: Toxin B subunit

I: Toxin B subunit

J: Toxin B subunit

K: Toxin B subunit

L: Toxin B subunit

M: Toxin B subunit

N: Toxin B subunit

O: Toxin B subunit

P: Toxin B subunit

Q: Toxin B subunit

R: Toxin B subunit

S: Toxin B subunit

T: Toxin B subunit

hetero molecules

A: Toxin B subunit

B: Toxin B subunit

C: Toxin B subunit

D: Toxin B subunit

E: Toxin B subunit

F: Toxin B subunit

G: Toxin B subunit

H: Toxin B subunit

I: Toxin B subunit

J: Toxin B subunit

K: Toxin B subunit

L: Toxin B subunit

M: Toxin B subunit

N: Toxin B subunit

O: Toxin B subunit

P: Toxin B subunit

Q: Toxin B subunit

R: Toxin B subunit

S: Toxin B subunit

T: Toxin B subunit

hetero molecules

A: Toxin B subunit

B: Toxin B subunit

C: Toxin B subunit

D: Toxin B subunit

E: Toxin B subunit

F: Toxin B subunit

G: Toxin B subunit

H: Toxin B subunit

I: Toxin B subunit

J: Toxin B subunit

K: Toxin B subunit

L: Toxin B subunit

M: Toxin B subunit

N: Toxin B subunit

O: Toxin B subunit

P: Toxin B subunit

Q: Toxin B subunit

R: Toxin B subunit

S: Toxin B subunit

T: Toxin B subunit

hetero molecules

A: Toxin B subunit

B: Toxin B subunit

C: Toxin B subunit

D: Toxin B subunit

E: Toxin B subunit

F: Toxin B subunit

G: Toxin B subunit

H: Toxin B subunit

I: Toxin B subunit

J: Toxin B subunit

K: Toxin B subunit

L: Toxin B subunit

M: Toxin B subunit

N: Toxin B subunit

O: Toxin B subunit

P: Toxin B subunit

Q: Toxin B subunit

R: Toxin B subunit

S: Toxin B subunit

T: Toxin B subunit

hetero molecules

Summary:

• defined by author
• Evidence: gel filtration, microscopy
• 1.69 MDa, 120 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	1,688,364	324
Polymers	1,665,588	120
Non-polymers	22,776	204
Water	2,162	120

Symmetry operations:

Type	Name	Symmetry operation	Number
identity operation	1_555	x,y,z	1
crystal symmetry operation	2_765	-y+2,x-y+1,z	1
crystal symmetry operation	3_675	-x+y+1,-x+2,z	1
crystal symmetry operation	4_774	-x+2,-y+2,z-1/2	1
crystal symmetry operation	5_564	y,-x+y+1,z-1/2	1
crystal symmetry operation	6_654	x-y+1,x,z-1/2	1

2

A: Toxin B subunit

B: Toxin B subunit

C: Toxin B subunit

D: Toxin B subunit

E: Toxin B subunit

hetero molecules

Summary:

• defined by author&software
• 70.3 kDa, 5 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	70,298	13
Polymers	69,400	5
Non-polymers	899	8
Water	90	5

Symmetry operations:

Type	Name	Symmetry operation	Number
identity operation	1_555	x,y,z	1

Calculated values:

Buried area	15410 Å2
ΔGint	-125 kcal/mol
Surface area	21450 Å2
Method	PISA

3

F: Toxin B subunit

G: Toxin B subunit

H: Toxin B subunit

I: Toxin B subunit

J: Toxin B subunit

hetero molecules

Summary:

• defined by author&software
• 70.4 kDa, 5 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	70,417	14
Polymers	69,400	5
Non-polymers	1,017	9
Water	90	5

Symmetry operations:

Type	Name	Symmetry operation	Number
identity operation	1_555	x,y,z	1

Calculated values:

Buried area	15850 Å2
ΔGint	-132 kcal/mol
Surface area	24240 Å2
Method	PISA

4

K: Toxin B subunit

L: Toxin B subunit

M: Toxin B subunit

N: Toxin B subunit

O: Toxin B subunit

hetero molecules

Summary:

• defined by author&software
• 70 kDa, 5 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	69,990	10
Polymers	69,400	5
Non-polymers	591	5
Water	90	5

Symmetry operations:

Type	Name	Symmetry operation	Number
identity operation	1_555	x,y,z	1

Calculated values:

Buried area	15520 Å2
ΔGint	-111 kcal/mol
Surface area	25250 Å2
Method	PISA

5

P: Toxin B subunit

Q: Toxin B subunit

R: Toxin B subunit

S: Toxin B subunit

T: Toxin B subunit

hetero molecules

Summary:

• defined by author&software
• 70.7 kDa, 5 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	70,688	17
Polymers	69,400	5
Non-polymers	1,289	12
Water	90	5

Symmetry operations:

Type	Name	Symmetry operation	Number
identity operation	1_555	x,y,z	1

Calculated values:

Buried area	16540 Å2
ΔGint	-172 kcal/mol
Surface area	21670 Å2
Method	PISA

Unit cell

Length a, b, c (Å)	179.160, 179.160, 192.020
Angle α, β, γ (deg.)	90.00, 90.00, 120.00
Int Tables number	173
Space group name H-M	P63

Noncrystallographic symmetry (NCS)

NCS domain:

ID	Ens-ID	Details
1	1	A
2	1	B
1	2	A
2	2	C
1	3	A
2	3	D
1	4	A
2	4	E
1	5	A
2	5	F
1	6	A
2	6	G
1	7	A
2	7	H
1	8	A
2	8	I
1	9	A
2	9	J
1	10	A
2	10	K
1	11	A
2	11	L
1	12	A
2	12	M
1	13	A
2	13	N
1	14	A
2	14	O
1	15	A
2	15	P
1	16	A
2	16	Q
1	17	A
2	17	R
1	18	A
2	18	S
1	19	A
2	19	T
1	20	B
2	20	C
1	21	B
2	21	D
1	22	B
2	22	E
1	23	B
2	23	F
1	24	B
2	24	G
1	25	B
2	25	H
1	26	B
2	26	I
1	27	B
2	27	J
1	28	B
2	28	K
1	29	B
2	29	L
1	30	B
2	30	M
1	31	B
2	31	N
1	32	B
2	32	O
1	33	B
2	33	P
1	34	B
2	34	Q
1	35	B
2	35	R
1	36	B
2	36	S
1	37	B
2	37	T
1	38	C
2	38	D
1	39	C
2	39	E
1	40	C
2	40	F
1	41	C
2	41	G
1	42	C
2	42	H
1	43	C
2	43	I
1	44	C
2	44	J
1	45	C
2	45	K
1	46	C
2	46	L
1	47	C
2	47	M
1	48	C
2	48	N
1	49	C
2	49	O
1	50	C
2	50	P
1	51	C
2	51	Q
1	52	C
2	52	R
1	53	C
2	53	S
1	54	C
2	54	T
1	55	D
2	55	E
1	56	D
2	56	F
1	57	D
2	57	G
1	58	D
2	58	H
1	59	D
2	59	I
1	60	D
2	60	J
1	61	D
2	61	K
1	62	D
2	62	L
1	63	D
2	63	M
1	64	D
2	64	N
1	65	D
2	65	O
1	66	D
2	66	P
1	67	D
2	67	Q
1	68	D
2	68	R
1	69	D
2	69	S
1	70	D
2	70	T
1	71	E
2	71	F
1	72	E
2	72	G
1	73	E
2	73	H
1	74	E
2	74	I
1	75	E
2	75	J
1	76	E
2	76	K
1	77	E
2	77	L
1	78	E
2	78	M
1	79	E
2	79	N
1	80	E
2	80	O
1	81	E
2	81	P
1	82	E
2	82	Q
1	83	E
2	83	R
1	84	E
2	84	S
1	85	E
2	85	T
1	86	F
2	86	G
1	87	F
2	87	H
1	88	F
2	88	I
1	89	F
2	89	J
1	90	F
2	90	K
1	91	F
2	91	L
1	92	F
2	92	M
1	93	F
2	93	N
1	94	F
2	94	O
1	95	F
2	95	P
1	96	F
2	96	Q
1	97	F
2	97	R
1	98	F
2	98	S
1	99	F
2	99	T
1	100	G
2	100	H
1	101	G
2	101	I
1	102	G
2	102	J
1	103	G
2	103	K
1	104	G
2	104	L
1	105	G
2	105	M
1	106	G
2	106	N
1	107	G
2	107	O
1	108	G
2	108	P
1	109	G
2	109	Q
1	110	G
2	110	R
1	111	G
2	111	S
1	112	G
2	112	T
1	113	H
2	113	I
1	114	H
2	114	J
1	115	H
2	115	K
1	116	H
2	116	L
1	117	H
2	117	M
1	118	H
2	118	N
1	119	H
2	119	O
1	120	H
2	120	P
1	121	H
2	121	Q
1	122	H
2	122	R
1	123	H
2	123	S
1	124	H
2	124	T
1	125	I
2	125	J
1	126	I
2	126	K
1	127	I
2	127	L
1	128	I
2	128	M
1	129	I
2	129	N
1	130	I
2	130	O
1	131	I
2	131	P
1	132	I
2	132	Q
1	133	I
2	133	R
1	134	I
2	134	S
1	135	I
2	135	T
1	136	J
2	136	K
1	137	J
2	137	L
1	138	J
2	138	M
1	139	J
2	139	N
1	140	J
2	140	O
1	141	J
2	141	P
1	142	J
2	142	Q
1	143	J
2	143	R
1	144	J
2	144	S
1	145	J
2	145	T
1	146	K
2	146	L
1	147	K
2	147	M
1	148	K
2	148	N
1	149	K
2	149	O
1	150	K
2	150	P
1	151	K
2	151	Q
1	152	K
2	152	R
1	153	K
2	153	S
1	154	K
2	154	T
1	155	L
2	155	M
1	156	L
2	156	N
1	157	L
2	157	O
1	158	L
2	158	P
1	159	L
2	159	Q
1	160	L
2	160	R
1	161	L
2	161	S
1	162	L
2	162	T
1	163	M
2	163	N
1	164	M
2	164	O
1	165	M
2	165	P
1	166	M
2	166	Q
1	167	M
2	167	R
1	168	M
2	168	S
1	169	M
2	169	T
1	170	N
2	170	O
1	171	N
2	171	P
1	172	N
2	172	Q
1	173	N
2	173	R
1	174	N
2	174	S
1	175	N
2	175	T
1	176	O
2	176	P
1	177	O
2	177	Q
1	178	O
2	178	R
1	179	O
2	179	S
1	180	O
2	180	T
1	181	P
2	181	Q
1	182	P
2	182	R
1	183	P
2	183	S
1	184	P
2	184	T
1	185	Q
2	185	R
1	186	Q
2	186	S
1	187	Q
2	187	T
1	188	R
2	188	S
1	189	R
2	189	T
1	190	S
2	190	T

NCS domain segments:

Component-ID: 0 / Beg auth comp-ID: THR / Beg label comp-ID: THR / Refine code: 0

Dom-ID	Ens-ID	End auth comp-ID	End label comp-ID	Auth asym-ID	Label asym-ID	Auth seq-ID	Label seq-ID
1	1	ALA	ALA	A	A	1 - 102	1 - 102
2	1	ALA	ALA	B	B	1 - 102	1 - 102
1	2	ASN	ASN	A	A	1 - 103	1 - 103
2	2	ASN	ASN	C	C	1 - 103	1 - 103
1	3	ALA	ALA	A	A	1 - 102	1 - 102
2	3	ALA	ALA	D	D	1 - 102	1 - 102
1	4	ASN	ASN	A	A	1 - 103	1 - 103
2	4	ASN	ASN	E	E	1 - 103	1 - 103
1	5	ASN	ASN	A	A	1 - 103	1 - 103
2	5	ASN	ASN	F	F	1 - 103	1 - 103
1	6	ASN	ASN	A	A	1 - 103	1 - 103
2	6	ASN	ASN	G	G	1 - 103	1 - 103
1	7	GLY	GLY	A	A	1 - 104	1 - 104
2	7	GLY	GLY	H	H	1 - 104	1 - 104
1	8	ALA	ALA	A	A	1 - 102	1 - 102
2	8	ALA	ALA	I	I	1 - 102	1 - 102
1	9	ASN	ASN	A	A	1 - 103	1 - 103
2	9	ASN	ASN	J	J	1 - 103	1 - 103
1	10	ALA	ALA	A	A	1 - 102	1 - 102
2	10	ALA	ALA	K	K	1 - 102	1 - 102
1	11	ASN	ASN	A	A	1 - 103	1 - 103
2	11	ASN	ASN	L	L	1 - 103	1 - 103
1	12	ASN	ASN	A	A	1 - 103	1 - 103
2	12	ASN	ASN	M	M	1 - 103	1 - 103
1	13	ASN	ASN	A	A	1 - 103	1 - 103
2	13	ASN	ASN	N	N	1 - 103	1 - 103
1	14	ASN	ASN	A	A	1 - 103	1 - 103
2	14	ASN	ASN	O	O	1 - 103	1 - 103
1	15	ASN	ASN	A	A	1 - 103	1 - 103
2	15	ASN	ASN	P	P	1 - 103	1 - 103
1	16	ALA	ALA	A	A	1 - 102	1 - 102
2	16	ALA	ALA	Q	Q	1 - 102	1 - 102
1	17	GLY	GLY	A	A	1 - 104	1 - 104
2	17	GLY	GLY	R	R	1 - 104	1 - 104
1	18	ALA	ALA	A	A	1 - 102	1 - 102
2	18	ALA	ALA	S	S	1 - 102	1 - 102
1	19	ALA	ALA	A	A	1 - 102	1 - 102
2	19	ALA	ALA	T	T	1 - 102	1 - 102
1	20	ASN	ASN	B	B	1 - 103	1 - 103
2	20	ASN	ASN	C	C	1 - 103	1 - 103
1	21	ASN	ASN	B	B	1 - 103	1 - 103
2	21	ASN	ASN	D	D	1 - 103	1 - 103
1	22	ALA	ALA	B	B	1 - 102	1 - 102
2	22	ALA	ALA	E	E	1 - 102	1 - 102
1	23	ALA	ALA	B	B	1 - 102	1 - 102
2	23	ALA	ALA	F	F	1 - 102	1 - 102
1	24	ALA	ALA	B	B	1 - 102	1 - 102
2	24	ALA	ALA	G	G	1 - 102	1 - 102
1	25	ALA	ALA	B	B	1 - 102	1 - 102
2	25	ALA	ALA	H	H	1 - 102	1 - 102
1	26	ASN	ASN	B	B	1 - 103	1 - 103
2	26	ASN	ASN	I	I	1 - 103	1 - 103
1	27	ALA	ALA	B	B	1 - 102	1 - 102
2	27	ALA	ALA	J	J	1 - 102	1 - 102
1	28	ASN	ASN	B	B	1 - 103	1 - 103
2	28	ASN	ASN	K	K	1 - 103	1 - 103
1	29	ALA	ALA	B	B	1 - 102	1 - 102
2	29	ALA	ALA	L	L	1 - 102	1 - 102
1	30	ALA	ALA	B	B	1 - 102	1 - 102
2	30	ALA	ALA	M	M	1 - 102	1 - 102
1	31	ALA	ALA	B	B	1 - 102	1 - 102
2	31	ALA	ALA	N	N	1 - 102	1 - 102
1	32	ALA	ALA	B	B	1 - 102	1 - 102
2	32	ALA	ALA	O	O	1 - 102	1 - 102
1	33	ALA	ALA	B	B	1 - 102	1 - 102
2	33	ALA	ALA	P	P	1 - 102	1 - 102
1	34	ASN	ASN	B	B	1 - 103	1 - 103
2	34	ASN	ASN	Q	Q	1 - 103	1 - 103
1	35	ALA	ALA	B	B	1 - 102	1 - 102
2	35	ALA	ALA	R	R	1 - 102	1 - 102
1	36	ASN	ASN	B	B	1 - 103	1 - 103
2	36	ASN	ASN	S	S	1 - 103	1 - 103
1	37	ASN	ASN	B	B	1 - 103	1 - 103
2	37	ASN	ASN	T	T	1 - 103	1 - 103
1	38	ASN	ASN	C	C	1 - 103	1 - 103
2	38	ASN	ASN	D	D	1 - 103	1 - 103
1	39	ALA	ALA	C	C	1 - 102	1 - 102
2	39	ALA	ALA	E	E	1 - 102	1 - 102
1	40	ALA	ALA	C	C	1 - 102	1 - 102
2	40	ALA	ALA	F	F	1 - 102	1 - 102
1	41	ALA	ALA	C	C	1 - 102	1 - 102
2	41	ALA	ALA	G	G	1 - 102	1 - 102
1	42	ASN	ASN	C	C	1 - 103	1 - 103
2	42	ASN	ASN	H	H	1 - 103	1 - 103
1	43	ASN	ASN	C	C	1 - 103	1 - 103
2	43	ASN	ASN	I	I	1 - 103	1 - 103
1	44	ALA	ALA	C	C	1 - 102	1 - 102
2	44	ALA	ALA	J	J	1 - 102	1 - 102
1	45	ASN	ASN	C	C	1 - 103	1 - 103
2	45	ASN	ASN	K	K	1 - 103	1 - 103
1	46	ALA	ALA	C	C	1 - 102	1 - 102
2	46	ALA	ALA	L	L	1 - 102	1 - 102
1	47	ALA	ALA	C	C	1 - 102	1 - 102
2	47	ALA	ALA	M	M	1 - 102	1 - 102
1	48	ALA	ALA	C	C	1 - 102	1 - 102
2	48	ALA	ALA	N	N	1 - 102	1 - 102
1	49	ALA	ALA	C	C	1 - 102	1 - 102
2	49	ALA	ALA	O	O	1 - 102	1 - 102
1	50	ALA	ALA	C	C	1 - 102	1 - 102
2	50	ALA	ALA	P	P	1 - 102	1 - 102
1	51	ASN	ASN	C	C	1 - 103	1 - 103
2	51	ASN	ASN	Q	Q	1 - 103	1 - 103
1	52	ASN	ASN	C	C	1 - 103	1 - 103
2	52	ASN	ASN	R	R	1 - 103	1 - 103
1	53	ASN	ASN	C	C	1 - 103	1 - 103
2	53	ASN	ASN	S	S	1 - 103	1 - 103
1	54	ASN	ASN	C	C	1 - 103	1 - 103
2	54	ASN	ASN	T	T	1 - 103	1 - 103
1	55	ALA	ALA	D	D	1 - 102	1 - 102
2	55	ALA	ALA	E	E	1 - 102	1 - 102
1	56	ALA	ALA	D	D	1 - 102	1 - 102
2	56	ALA	ALA	F	F	1 - 102	1 - 102
1	57	ALA	ALA	D	D	1 - 102	1 - 102
2	57	ALA	ALA	G	G	1 - 102	1 - 102
1	58	ALA	ALA	D	D	1 - 102	1 - 102
2	58	ALA	ALA	H	H	1 - 102	1 - 102
1	59	ASN	ASN	D	D	1 - 103	1 - 103
2	59	ASN	ASN	I	I	1 - 103	1 - 103
1	60	ALA	ALA	D	D	1 - 102	1 - 102
2	60	ALA	ALA	J	J	1 - 102	1 - 102
1	61	ASN	ASN	D	D	1 - 103	1 - 103
2	61	ASN	ASN	K	K	1 - 103	1 - 103
1	62	ALA	ALA	D	D	1 - 102	1 - 102
2	62	ALA	ALA	L	L	1 - 102	1 - 102
1	63	ALA	ALA	D	D	1 - 102	1 - 102
2	63	ALA	ALA	M	M	1 - 102	1 - 102
1	64	ALA	ALA	D	D	1 - 102	1 - 102
2	64	ALA	ALA	N	N	1 - 102	1 - 102
1	65	ALA	ALA	D	D	1 - 102	1 - 102
2	65	ALA	ALA	O	O	1 - 102	1 - 102
1	66	ALA	ALA	D	D	1 - 102	1 - 102
2	66	ALA	ALA	P	P	1 - 102	1 - 102
1	67	ASN	ASN	D	D	1 - 103	1 - 103
2	67	ASN	ASN	Q	Q	1 - 103	1 - 103
1	68	ALA	ALA	D	D	1 - 102	1 - 102
2	68	ALA	ALA	R	R	1 - 102	1 - 102
1	69	ASN	ASN	D	D	1 - 103	1 - 103
2	69	ASN	ASN	S	S	1 - 103	1 - 103
1	70	ASN	ASN	D	D	1 - 103	1 - 103
2	70	ASN	ASN	T	T	1 - 103	1 - 103
1	71	GLU	GLU	E	E	1 - 123	1 - 123
2	71	GLU	GLU	F	F	1 - 123	1 - 123
1	72	GLU	GLU	E	E	1 - 123	1 - 123
2	72	GLU	GLU	G	G	1 - 123	1 - 123
1	73	ASN	ASN	E	E	1 - 103	1 - 103
2	73	ASN	ASN	H	H	1 - 103	1 - 103
1	74	ALA	ALA	E	E	1 - 102	1 - 102
2	74	ALA	ALA	I	I	1 - 102	1 - 102
1	75	GLU	GLU	E	E	1 - 123	1 - 123
2	75	GLU	GLU	J	J	1 - 123	1 - 123
1	76	ALA	ALA	E	E	1 - 102	1 - 102
2	76	ALA	ALA	K	K	1 - 102	1 - 102
1	77	GLU	GLU	E	E	1 - 123	1 - 123
2	77	GLU	GLU	L	L	1 - 123	1 - 123
1	78	GLU	GLU	E	E	1 - 123	1 - 123
2	78	GLU	GLU	M	M	1 - 123	1 - 123
1	79	GLU	GLU	E	E	1 - 123	1 - 123
2	79	GLU	GLU	N	N	1 - 123	1 - 123
1	80	GLU	GLU	E	E	1 - 123	1 - 123
2	80	GLU	GLU	O	O	1 - 123	1 - 123
1	81	GLU	GLU	E	E	1 - 123	1 - 123
2	81	GLU	GLU	P	P	1 - 123	1 - 123
1	82	ALA	ALA	E	E	1 - 102	1 - 102
2	82	ALA	ALA	Q	Q	1 - 102	1 - 102
1	83	ASN	ASN	E	E	1 - 103	1 - 103
2	83	ASN	ASN	R	R	1 - 103	1 - 103
1	84	ALA	ALA	E	E	1 - 102	1 - 102
2	84	ALA	ALA	S	S	1 - 102	1 - 102
1	85	ALA	ALA	E	E	1 - 102	1 - 102
2	85	ALA	ALA	T	T	1 - 102	1 - 102
1	86	GLU	GLU	F	F	1 - 123	1 - 123
2	86	GLU	GLU	G	G	1 - 123	1 - 123
1	87	ASN	ASN	F	F	1 - 103	1 - 103
2	87	ASN	ASN	H	H	1 - 103	1 - 103
1	88	ALA	ALA	F	F	1 - 102	1 - 102
2	88	ALA	ALA	I	I	1 - 102	1 - 102
1	89	GLU	GLU	F	F	1 - 123	1 - 123
2	89	GLU	GLU	J	J	1 - 123	1 - 123
1	90	ALA	ALA	F	F	1 - 102	1 - 102
2	90	ALA	ALA	K	K	1 - 102	1 - 102
1	91	GLU	GLU	F	F	1 - 123	1 - 123
2	91	GLU	GLU	L	L	1 - 123	1 - 123
1	92	GLU	GLU	F	F	1 - 123	1 - 123
2	92	GLU	GLU	M	M	1 - 123	1 - 123
1	93	GLU	GLU	F	F	1 - 123	1 - 123
2	93	GLU	GLU	N	N	1 - 123	1 - 123
1	94	GLU	GLU	F	F	1 - 123	1 - 123
2	94	GLU	GLU	O	O	1 - 123	1 - 123
1	95	GLU	GLU	F	F	1 - 123	1 - 123
2	95	GLU	GLU	P	P	1 - 123	1 - 123
1	96	ALA	ALA	F	F	1 - 102	1 - 102
2	96	ALA	ALA	Q	Q	1 - 102	1 - 102
1	97	ASN	ASN	F	F	1 - 103	1 - 103
2	97	ASN	ASN	R	R	1 - 103	1 - 103
1	98	ALA	ALA	F	F	1 - 102	1 - 102
2	98	ALA	ALA	S	S	1 - 102	1 - 102
1	99	ALA	ALA	F	F	1 - 102	1 - 102
2	99	ALA	ALA	T	T	1 - 102	1 - 102
1	100	ASN	ASN	G	G	1 - 103	1 - 103
2	100	ASN	ASN	H	H	1 - 103	1 - 103
1	101	ALA	ALA	G	G	1 - 102	1 - 102
2	101	ALA	ALA	I	I	1 - 102	1 - 102
1	102	GLU	GLU	G	G	1 - 123	1 - 123
2	102	GLU	GLU	J	J	1 - 123	1 - 123
1	103	ALA	ALA	G	G	1 - 102	1 - 102
2	103	ALA	ALA	K	K	1 - 102	1 - 102
1	104	GLU	GLU	G	G	1 - 123	1 - 123
2	104	GLU	GLU	L	L	1 - 123	1 - 123
1	105	GLU	GLU	G	G	1 - 123	1 - 123
2	105	GLU	GLU	M	M	1 - 123	1 - 123
1	106	GLU	GLU	G	G	1 - 123	1 - 123
2	106	GLU	GLU	N	N	1 - 123	1 - 123
1	107	GLU	GLU	G	G	1 - 123	1 - 123
2	107	GLU	GLU	O	O	1 - 123	1 - 123
1	108	GLU	GLU	G	G	1 - 123	1 - 123
2	108	GLU	GLU	P	P	1 - 123	1 - 123
1	109	ALA	ALA	G	G	1 - 102	1 - 102
2	109	ALA	ALA	Q	Q	1 - 102	1 - 102
1	110	ASN	ASN	G	G	1 - 103	1 - 103
2	110	ASN	ASN	R	R	1 - 103	1 - 103
1	111	ALA	ALA	G	G	1 - 102	1 - 102
2	111	ALA	ALA	S	S	1 - 102	1 - 102
1	112	ALA	ALA	G	G	1 - 102	1 - 102
2	112	ALA	ALA	T	T	1 - 102	1 - 102
1	113	ALA	ALA	H	H	1 - 102	1 - 102
2	113	ALA	ALA	I	I	1 - 102	1 - 102
1	114	ASN	ASN	H	H	1 - 103	1 - 103
2	114	ASN	ASN	J	J	1 - 103	1 - 103
1	115	ALA	ALA	H	H	1 - 102	1 - 102
2	115	ALA	ALA	K	K	1 - 102	1 - 102
1	116	ASN	ASN	H	H	1 - 103	1 - 103
2	116	ASN	ASN	L	L	1 - 103	1 - 103
1	117	ASN	ASN	H	H	1 - 103	1 - 103
2	117	ASN	ASN	M	M	1 - 103	1 - 103
1	118	ASN	ASN	H	H	1 - 103	1 - 103
2	118	ASN	ASN	N	N	1 - 103	1 - 103
1	119	ASN	ASN	H	H	1 - 103	1 - 103
2	119	ASN	ASN	O	O	1 - 103	1 - 103
1	120	ASN	ASN	H	H	1 - 103	1 - 103
2	120	ASN	ASN	P	P	1 - 103	1 - 103
1	121	ALA	ALA	H	H	1 - 102	1 - 102
2	121	ALA	ALA	Q	Q	1 - 102	1 - 102
1	122	GLY	GLY	H	H	1 - 104	1 - 104
2	122	GLY	GLY	R	R	1 - 104	1 - 104
1	123	ALA	ALA	H	H	1 - 102	1 - 102
2	123	ALA	ALA	S	S	1 - 102	1 - 102
1	124	ALA	ALA	H	H	1 - 102	1 - 102
2	124	ALA	ALA	T	T	1 - 102	1 - 102
1	125	ALA	ALA	I	I	1 - 102	1 - 102
2	125	ALA	ALA	J	J	1 - 102	1 - 102
1	126	ASN	ASN	I	I	1 - 103	1 - 103
2	126	ASN	ASN	K	K	1 - 103	1 - 103
1	127	ALA	ALA	I	I	1 - 102	1 - 102
2	127	ALA	ALA	L	L	1 - 102	1 - 102
1	128	ALA	ALA	I	I	1 - 102	1 - 102
2	128	ALA	ALA	M	M	1 - 102	1 - 102
1	129	ALA	ALA	I	I	1 - 102	1 - 102
2	129	ALA	ALA	N	N	1 - 102	1 - 102
1	130	ALA	ALA	I	I	1 - 102	1 - 102
2	130	ALA	ALA	O	O	1 - 102	1 - 102
1	131	ALA	ALA	I	I	1 - 102	1 - 102
2	131	ALA	ALA	P	P	1 - 102	1 - 102
1	132	ASN	ASN	I	I	1 - 103	1 - 103
2	132	ASN	ASN	Q	Q	1 - 103	1 - 103
1	133	ALA	ALA	I	I	1 - 102	1 - 102
2	133	ALA	ALA	R	R	1 - 102	1 - 102
1	134	ASN	ASN	I	I	1 - 103	1 - 103
2	134	ASN	ASN	S	S	1 - 103	1 - 103
1	135	ASN	ASN	I	I	1 - 103	1 - 103
2	135	ASN	ASN	T	T	1 - 103	1 - 103
1	136	ALA	ALA	J	J	1 - 102	1 - 102
2	136	ALA	ALA	K	K	1 - 102	1 - 102
1	137	GLU	GLU	J	J	1 - 123	1 - 123
2	137	GLU	GLU	L	L	1 - 123	1 - 123
1	138	GLU	GLU	J	J	1 - 123	1 - 123
2	138	GLU	GLU	M	M	1 - 123	1 - 123
1	139	GLU	GLU	J	J	1 - 123	1 - 123
2	139	GLU	GLU	N	N	1 - 123	1 - 123
1	140	GLU	GLU	J	J	1 - 123	1 - 123
2	140	GLU	GLU	O	O	1 - 123	1 - 123
1	141	GLU	GLU	J	J	1 - 123	1 - 123
2	141	GLU	GLU	P	P	1 - 123	1 - 123
1	142	ALA	ALA	J	J	1 - 102	1 - 102
2	142	ALA	ALA	Q	Q	1 - 102	1 - 102
1	143	ASN	ASN	J	J	1 - 103	1 - 103
2	143	ASN	ASN	R	R	1 - 103	1 - 103
1	144	ALA	ALA	J	J	1 - 102	1 - 102
2	144	ALA	ALA	S	S	1 - 102	1 - 102
1	145	ALA	ALA	J	J	1 - 102	1 - 102
2	145	ALA	ALA	T	T	1 - 102	1 - 102
1	146	ALA	ALA	K	K	1 - 102	1 - 102
2	146	ALA	ALA	L	L	1 - 102	1 - 102
1	147	ALA	ALA	K	K	1 - 102	1 - 102
2	147	ALA	ALA	M	M	1 - 102	1 - 102
1	148	ALA	ALA	K	K	1 - 102	1 - 102
2	148	ALA	ALA	N	N	1 - 102	1 - 102
1	149	ALA	ALA	K	K	1 - 102	1 - 102
2	149	ALA	ALA	O	O	1 - 102	1 - 102
1	150	ALA	ALA	K	K	1 - 102	1 - 102
2	150	ALA	ALA	P	P	1 - 102	1 - 102
1	151	ASN	ASN	K	K	1 - 103	1 - 103
2	151	ASN	ASN	Q	Q	1 - 103	1 - 103
1	152	ALA	ALA	K	K	1 - 102	1 - 102
2	152	ALA	ALA	R	R	1 - 102	1 - 102
1	153	ASN	ASN	K	K	1 - 103	1 - 103
2	153	ASN	ASN	S	S	1 - 103	1 - 103
1	154	ASN	ASN	K	K	1 - 103	1 - 103
2	154	ASN	ASN	T	T	1 - 103	1 - 103
1	155	GLU	GLU	L	L	1 - 123	1 - 123
2	155	GLU	GLU	M	M	1 - 123	1 - 123
1	156	GLU	GLU	L	L	1 - 123	1 - 123
2	156	GLU	GLU	N	N	1 - 123	1 - 123
1	157	GLU	GLU	L	L	1 - 123	1 - 123
2	157	GLU	GLU	O	O	1 - 123	1 - 123
1	158	GLU	GLU	L	L	1 - 123	1 - 123
2	158	GLU	GLU	P	P	1 - 123	1 - 123
1	159	ALA	ALA	L	L	1 - 102	1 - 102
2	159	ALA	ALA	Q	Q	1 - 102	1 - 102
1	160	ASN	ASN	L	L	1 - 103	1 - 103
2	160	ASN	ASN	R	R	1 - 103	1 - 103
1	161	ALA	ALA	L	L	1 - 102	1 - 102
2	161	ALA	ALA	S	S	1 - 102	1 - 102
1	162	ALA	ALA	L	L	1 - 102	1 - 102
2	162	ALA	ALA	T	T	1 - 102	1 - 102
1	163	GLU	GLU	M	M	1 - 123	1 - 123
2	163	GLU	GLU	N	N	1 - 123	1 - 123
1	164	GLU	GLU	M	M	1 - 123	1 - 123
2	164	GLU	GLU	O	O	1 - 123	1 - 123
1	165	GLU	GLU	M	M	1 - 123	1 - 123
2	165	GLU	GLU	P	P	1 - 123	1 - 123
1	166	ALA	ALA	M	M	1 - 102	1 - 102
2	166	ALA	ALA	Q	Q	1 - 102	1 - 102
1	167	ASN	ASN	M	M	1 - 103	1 - 103
2	167	ASN	ASN	R	R	1 - 103	1 - 103
1	168	ALA	ALA	M	M	1 - 102	1 - 102
2	168	ALA	ALA	S	S	1 - 102	1 - 102
1	169	ALA	ALA	M	M	1 - 102	1 - 102
2	169	ALA	ALA	T	T	1 - 102	1 - 102
1	170	GLU	GLU	N	N	1 - 123	1 - 123
2	170	GLU	GLU	O	O	1 - 123	1 - 123
1	171	GLU	GLU	N	N	1 - 123	1 - 123
2	171	GLU	GLU	P	P	1 - 123	1 - 123
1	172	ALA	ALA	N	N	1 - 102	1 - 102
2	172	ALA	ALA	Q	Q	1 - 102	1 - 102
1	173	ASN	ASN	N	N	1 - 103	1 - 103
2	173	ASN	ASN	R	R	1 - 103	1 - 103
1	174	ALA	ALA	N	N	1 - 102	1 - 102
2	174	ALA	ALA	S	S	1 - 102	1 - 102
1	175	ALA	ALA	N	N	1 - 102	1 - 102
2	175	ALA	ALA	T	T	1 - 102	1 - 102
1	176	GLU	GLU	O	O	1 - 123	1 - 123
2	176	GLU	GLU	P	P	1 - 123	1 - 123
1	177	ALA	ALA	O	O	1 - 102	1 - 102
2	177	ALA	ALA	Q	Q	1 - 102	1 - 102
1	178	ASN	ASN	O	O	1 - 103	1 - 103
2	178	ASN	ASN	R	R	1 - 103	1 - 103
1	179	ALA	ALA	O	O	1 - 102	1 - 102
2	179	ALA	ALA	S	S	1 - 102	1 - 102
1	180	ALA	ALA	O	O	1 - 102	1 - 102
2	180	ALA	ALA	T	T	1 - 102	1 - 102
1	181	ALA	ALA	P	P	1 - 102	1 - 102
2	181	ALA	ALA	Q	Q	1 - 102	1 - 102
1	182	ASN	ASN	P	P	1 - 103	1 - 103
2	182	ASN	ASN	R	R	1 - 103	1 - 103
1	183	ALA	ALA	P	P	1 - 102	1 - 102
2	183	ALA	ALA	S	S	1 - 102	1 - 102
1	184	ALA	ALA	P	P	1 - 102	1 - 102
2	184	ALA	ALA	T	T	1 - 102	1 - 102
1	185	ALA	ALA	Q	Q	1 - 102	1 - 102
2	185	ALA	ALA	R	R	1 - 102	1 - 102
1	186	ASN	ASN	Q	Q	1 - 103	1 - 103
2	186	ASN	ASN	S	S	1 - 103	1 - 103
1	187	ASN	ASN	Q	Q	1 - 103	1 - 103
2	187	ASN	ASN	T	T	1 - 103	1 - 103
1	188	ALA	ALA	R	R	1 - 102	1 - 102
2	188	ALA	ALA	S	S	1 - 102	1 - 102
1	189	ALA	ALA	R	R	1 - 102	1 - 102
2	189	ALA	ALA	T	T	1 - 102	1 - 102
1	190	ASN	ASN	S	S	1 - 103	1 - 103
2	190	ASN	ASN	T	T	1 - 103	1 - 103

NCS ensembles :

ID
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
116
117
118
119
120
121
122
123
124
125
126
127
128
129
130
131
132
133
134
135
136
137
138
139
140
141
142
143
144
145
146
147
148
149
150
151
152
153
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
169
170
171
172
173
174
175
176
177
178
179
180
181
182
183
184
185
186
187
188
189
190

Components

#1: Protein

A B C D E F G H I J K L M N O P Q R S T
Toxin B subunit

Details:

Mass: 13879.902 Da / Num. of mol.: 20
Source method: isolated from a genetically manipulated source
Source: (gene. exp.) Vibrio cholerae (bacteria) / Gene: CTB / Plasmid: pSAB2.2 / Production host: Escherichia coli BL21(DE3) (bacteria) / Variant (production host): C41 / References: UniProt: Q7X2D2, UniProt: P01556*PLUS

#2: Chemical

A-201 D-201 F-201 I-201 P-201 Q-201
ChemComp-PO4 / PHOSPHATE ION / Phosphate

Details:

Mass: 94.971 Da / Num. of mol.: 6 / Source method: obtained synthetically / Formula: PO₄

#3: Chemical

A-202 A-203 B-201 B-202 D-202 D-203 G-201 G-202 H-201 H-202 H-203 J-201 J-202 L-201 M-201 N-201 O-201 O-202 P-202 P-203 ...
ChemComp-MPD / (4S)-2-METHYL-2,4-PENTANEDIOL / 2-Methyl-2,4-pentanediol

Details:

Mass: 118.174 Da / Num. of mol.: 27 / Source method: obtained synthetically / Formula: C₆H₁₄O₂ / Comment: precipitant*YM

#4: Chemical

T-202 ChemComp-CL / CHLORIDE ION / Chloride

Details:

Mass: 35.453 Da / Num. of mol.: 1 / Source method: obtained synthetically / Formula: Cl

#5: Water

ChemComp-HOH / water / Water

Details:

Mass: 18.015 Da / Num. of mol.: 584 / Source method: isolated from a natural source / Formula: H₂O

Experimental details

Experiment

• Experiment: Method: X-RAY DIFFRACTION / Number of used crystals: 1

Sample preparation

• Crystal: Density Matthews: 3.54 ų/Da / Density % sol: 65.24 %
• Crystal grow: Temperature: 293 K / Method: vapor diffusion, hanging drop / pH: 8.5 ; Details: Hampton Crystal Screen 2 condition #43: 0.2 M Ammonium Phosphate monobasic, 0.1 M Tris (pH 8.5), 50% v/v (+/-)-2-Methyl-2,4-pentanediol.

Data collection

• Diffraction: Mean temperature: 100 K
• Diffraction source: Source: SYNCHROTRON / Site: Diamond / Beamline: I24 / Wavelength: 0.96862 Å
• Detector: Type: DECTRIS PILATUS 6M / Detector: PIXEL / Date: May 24, 2014
• Radiation: Protocol: SINGLE WAVELENGTH / Monochromatic (M) / Laue (L): M / Scattering type: x-ray
• Radiation wavelength: Wavelength: 0.96862 Å / Relative weight: 1
• Reflection: Resolution: 2.45→37.28 Å / Num. obs: 127892 / % possible obs: 100 % / Redundancy: 10.2 % / CC_1/2: 0.999 / R_merge(I) obs: 0.092 / R_pim(I) all: 0.03 / R_rim(I) all: 0.097 / Net I/σ(I): 19
• Reflection shell: Resolution: 2.45→2.51 Å / Redundancy: 8.4 % / R_merge(I) obs: 0.698 / Mean I/σ(I) obs: 3.2 / Num. unique obs: 9402 / CC_1/2: 0.864 / R_pim(I) all: 0.346 / R_rim(I) all: 0.744 / % possible all: 100

Processing

Software

Name	Version	Classification
REFMAC	5.8.0232	refinement
PDB_EXTRACT	3.22	data extraction
xia2		data reduction
Aimless	0.2.17	data scaling
MOLREP		phasing

Refinement

Method to determine structure: MOLECULAR REPLACEMENT
Starting model: 3CHB

3chb

Resolution: 2.45→37.28 Å / Cor.coef. F_o:F_c: 0.947 / Cor.coef. F_o:F_c free: 0.935 / SU B: 14.984 / SU ML: 0.174 / Cross valid method: THROUGHOUT / ESU R: 0.295 / ESU R Free: 0.205
Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. Each CTB pentamer (residues 1-103, chains ABCDE, FGHIJ, KLMNO, PQRST) and each of the three triple helices (residues 104-124, chains EFG, JLM, NOP) was described with a separate single TLS group. Restrained refinement used REFMAC automatically generated local NCS restraints.

	Rfactor	Num. reflection	% reflection	Selection details
Rfree	0.21378	6304	4.9 %	RANDOM
Rwork	0.19548	-	-	-
obs	0.19639	121547	99.96 %	-

• Solvent computation: Ion probe radii: 0.8 Å / Shrinkage radii: 0.8 Å / VDW probe radii: 1.2 Å

Displacement parameters

B_iso mean: 55.917 Ų

	Baniso -1	Baniso -2	Baniso -3
1-	0.97 Å2	0.48 Å2	0 Å2
2-	-	0.97 Å2	0 Å2
3-	-	-	-3.14 Å2

Refinement step

Cycle: 1 / Resolution: 2.45→37.28 Å

	Protein	Nucleic acid	Ligand	Solvent	Total
Num. atoms	17187	0	247	584	18018

Refine LS restraints

Refine-ID	Type	Dev ideal	Dev ideal target	Number
X-RAY DIFFRACTION	r_bond_refined_d	0.014	0.013	17740
X-RAY DIFFRACTION	r_bond_other_d	0.001	0.017	16513
X-RAY DIFFRACTION	r_angle_refined_deg	1.794	1.65	24057
X-RAY DIFFRACTION	r_angle_other_deg	1.367	1.578	38256
X-RAY DIFFRACTION	r_dihedral_angle_1_deg	15.048	5.199	2266
X-RAY DIFFRACTION	r_dihedral_angle_2_deg	38.244	24.212	793
X-RAY DIFFRACTION	r_dihedral_angle_3_deg	16.289	15	3049
X-RAY DIFFRACTION	r_dihedral_angle_4_deg	26.331	15	61
X-RAY DIFFRACTION	r_chiral_restr	0.083	0.2	2597
X-RAY DIFFRACTION	r_gen_planes_refined	0.009	0.02	20919
X-RAY DIFFRACTION	r_gen_planes_other	0.001	0.02	3331
X-RAY DIFFRACTION	r_nbd_refined
X-RAY DIFFRACTION	r_nbd_other
X-RAY DIFFRACTION	r_nbtor_refined
X-RAY DIFFRACTION	r_nbtor_other
X-RAY DIFFRACTION	r_xyhbond_nbd_refined
X-RAY DIFFRACTION	r_xyhbond_nbd_other
X-RAY DIFFRACTION	r_metal_ion_refined
X-RAY DIFFRACTION	r_metal_ion_other
X-RAY DIFFRACTION	r_symmetry_vdw_refined
X-RAY DIFFRACTION	r_symmetry_vdw_other
X-RAY DIFFRACTION	r_symmetry_hbond_refined
X-RAY DIFFRACTION	r_symmetry_hbond_other
X-RAY DIFFRACTION	r_symmetry_metal_ion_refined
X-RAY DIFFRACTION	r_symmetry_metal_ion_other
X-RAY DIFFRACTION	r_mcbond_it	1.442	1.73	8949
X-RAY DIFFRACTION	r_mcbond_other	1.441	1.729	8948
X-RAY DIFFRACTION	r_mcangle_it	2.423	2.586	11157
X-RAY DIFFRACTION	r_mcangle_other	2.423	2.586	11158
X-RAY DIFFRACTION	r_scbond_it	2.157	2.031	8791
X-RAY DIFFRACTION	r_scbond_other	2.157	2.031	8792
X-RAY DIFFRACTION	r_scangle_it
X-RAY DIFFRACTION	r_scangle_other	3.221	2.954	12900
X-RAY DIFFRACTION	r_long_range_B_refined	6.508	21.029	18816
X-RAY DIFFRACTION	r_long_range_B_other	6.508	21.032	18817
X-RAY DIFFRACTION	r_rigid_bond_restr
X-RAY DIFFRACTION	r_sphericity_free
X-RAY DIFFRACTION	r_sphericity_bonded

Refine LS restraints NCS

Refine-ID: X-RAY DIFFRACTION / Type: interatomic distance / Weight position: 0.05

Ens-ID	Dom-ID	Auth asym-ID	Number	Rms dev position (Å)
1	1	A	3074	0.06
1	2	B	3074	0.06
2	1	A	2860	0.08
2	2	C	2860	0.08
3	1	A	3076	0.07
3	2	D	3076	0.07
4	1	A	3067	0.06
4	2	E	3067	0.06
5	1	A	3063	0.06
5	2	F	3063	0.06
6	1	A	3090	0.06
6	2	G	3090	0.06
7	1	A	3108	0.06
7	2	H	3108	0.06
8	1	A	3081	0.05
8	2	I	3081	0.05
9	1	A	3113	0.06
9	2	J	3113	0.06
10	1	A	3067	0.06
10	2	K	3067	0.06
11	1	A	3093	0.07
11	2	L	3093	0.07
12	1	A	3084	0.06
12	2	M	3084	0.06
13	1	A	3030	0.08
13	2	N	3030	0.08
14	1	A	3072	0.06
14	2	O	3072	0.06
15	1	A	3119	0.06
15	2	P	3119	0.06
16	1	A	3111	0.04
16	2	Q	3111	0.04
17	1	A	3134	0.05
17	2	R	3134	0.05
18	1	A	3050	0.07
18	2	S	3050	0.07
19	1	A	3107	0.05
19	2	T	3107	0.05
20	1	B	2865	0.08
20	2	C	2865	0.08
21	1	B	3088	0.07
21	2	D	3088	0.07
22	1	B	3067	0.06
22	2	E	3067	0.06
23	1	B	3051	0.07
23	2	F	3051	0.07
24	1	B	3053	0.06
24	2	G	3053	0.06
25	1	B	3100	0.05
25	2	H	3100	0.05
26	1	B	3108	0.06
26	2	I	3108	0.06
27	1	B	3072	0.06
27	2	J	3072	0.06
28	1	B	3096	0.07
28	2	K	3096	0.07
29	1	B	3053	0.07
29	2	L	3053	0.07
30	1	B	3075	0.06
30	2	M	3075	0.06
31	1	B	3016	0.08
31	2	N	3016	0.08
32	1	B	3080	0.06
32	2	O	3080	0.06
33	1	B	3075	0.05
33	2	P	3075	0.05
34	1	B	3088	0.06
34	2	Q	3088	0.06
35	1	B	3078	0.06
35	2	R	3078	0.06
36	1	B	3065	0.08
36	2	S	3065	0.08
37	1	B	3095	0.07
37	2	T	3095	0.07
38	1	C	2853	0.08
38	2	D	2853	0.08
39	1	C	2821	0.08
39	2	E	2821	0.08
40	1	C	2829	0.09
40	2	F	2829	0.09
41	1	C	2847	0.07
41	2	G	2847	0.07
42	1	C	2866	0.08
42	2	H	2866	0.08
43	1	C	2860	0.08
43	2	I	2860	0.08
44	1	C	2860	0.07
44	2	J	2860	0.07
45	1	C	2863	0.08
45	2	K	2863	0.08
46	1	C	2820	0.09
46	2	L	2820	0.09
47	1	C	2840	0.07
47	2	M	2840	0.07
48	1	C	2787	0.09
48	2	N	2787	0.09
49	1	C	2860	0.07
49	2	O	2860	0.07
50	1	C	2847	0.07
50	2	P	2847	0.07
51	1	C	2868	0.08
51	2	Q	2868	0.08
52	1	C	2856	0.08
52	2	R	2856	0.08
53	1	C	2873	0.08
53	2	S	2873	0.08
54	1	C	2865	0.08
54	2	T	2865	0.08
55	1	D	3026	0.07
55	2	E	3026	0.07
56	1	D	3019	0.08
56	2	F	3019	0.08
57	1	D	3055	0.07
57	2	G	3055	0.07
58	1	D	3074	0.06
58	2	H	3074	0.06
59	1	D	3073	0.07
59	2	I	3073	0.07
60	1	D	3086	0.07
60	2	J	3086	0.07
61	1	D	3082	0.06
61	2	K	3082	0.06
62	1	D	3062	0.08
62	2	L	3062	0.08
63	1	D	3056	0.07
63	2	M	3056	0.07
64	1	D	2994	0.09
64	2	N	2994	0.09
65	1	D	3050	0.06
65	2	O	3050	0.06
66	1	D	3073	0.06
66	2	P	3073	0.06
67	1	D	3115	0.06
67	2	Q	3115	0.06
68	1	D	3073	0.07
68	2	R	3073	0.07
69	1	D	3049	0.08
69	2	S	3049	0.08
70	1	D	3106	0.07
70	2	T	3106	0.07
71	1	E	3393	0.06
71	2	F	3393	0.06
72	1	E	3386	0.07
72	2	G	3386	0.07
73	1	E	3095	0.06
73	2	H	3095	0.06
74	1	E	3071	0.05
74	2	I	3071	0.05
75	1	E	3405	0.06
75	2	J	3405	0.06
76	1	E	3071	0.05
76	2	K	3071	0.05
77	1	E	3399	0.07
77	2	L	3399	0.07
78	1	E	3404	0.06
78	2	M	3404	0.06
79	1	E	3356	0.07
79	2	N	3356	0.07
80	1	E	3401	0.06
80	2	O	3401	0.06
81	1	E	3426	0.06
81	2	P	3426	0.06
82	1	E	3054	0.05
82	2	Q	3054	0.05
83	1	E	3071	0.05
83	2	R	3071	0.05
84	1	E	3017	0.07
84	2	S	3017	0.07
85	1	E	3064	0.05
85	2	T	3064	0.05
86	1	F	3363	0.08
86	2	G	3363	0.08
87	1	F	3078	0.06
87	2	H	3078	0.06
88	1	F	3058	0.06
88	2	I	3058	0.06
89	1	F	3387	0.07
89	2	J	3387	0.07
90	1	F	3052	0.07
90	2	K	3052	0.07
91	1	F	3381	0.09
91	2	L	3381	0.09
92	1	F	3392	0.07
92	2	M	3392	0.07
93	1	F	3404	0.06
93	2	N	3404	0.06
94	1	F	3388	0.07
94	2	O	3388	0.07
95	1	F	3396	0.08
95	2	P	3396	0.08
96	1	F	3043	0.05
96	2	Q	3043	0.05
97	1	F	3066	0.05
97	2	R	3066	0.05
98	1	F	3007	0.07
98	2	S	3007	0.07
99	1	F	3055	0.06
99	2	T	3055	0.06
100	1	G	3075	0.07
100	2	H	3075	0.07
101	1	G	3057	0.06
101	2	I	3057	0.06
102	1	G	3432	0.06
102	2	J	3432	0.06
103	1	G	3051	0.07
103	2	K	3051	0.07
104	1	G	3397	0.08
104	2	L	3397	0.08
105	1	G	3405	0.06
105	2	M	3405	0.06
106	1	G	3334	0.08
106	2	N	3334	0.08
107	1	G	3443	0.04
107	2	O	3443	0.04
108	1	G	3426	0.07
108	2	P	3426	0.07
109	1	G	3078	0.05
109	2	Q	3078	0.05
110	1	G	3079	0.06
110	2	R	3079	0.06
111	1	G	3037	0.08
111	2	S	3037	0.08
112	1	G	3067	0.07
112	2	T	3067	0.07
113	1	H	3099	0.05
113	2	I	3099	0.05
114	1	H	3099	0.06
114	2	J	3099	0.06
115	1	H	3098	0.05
115	2	K	3098	0.05
116	1	H	3084	0.06
116	2	L	3084	0.06
117	1	H	3103	0.06
117	2	M	3103	0.06
118	1	H	3048	0.08
118	2	N	3048	0.08
119	1	H	3100	0.06
119	2	O	3100	0.06
120	1	H	3107	0.05
120	2	P	3107	0.05
121	1	H	3085	0.05
121	2	Q	3085	0.05
122	1	H	3100	0.05
122	2	R	3100	0.05
123	1	H	3051	0.07
123	2	S	3051	0.07
124	1	H	3094	0.05
124	2	T	3094	0.05
125	1	I	3076	0.05
125	2	J	3076	0.05
126	1	I	3098	0.07
126	2	K	3098	0.07
127	1	I	3075	0.05
127	2	L	3075	0.05
128	1	I	3079	0.05
128	2	M	3079	0.05
129	1	I	3030	0.07
129	2	N	3030	0.07
130	1	I	3079	0.06
130	2	O	3079	0.06
131	1	I	3077	0.06
131	2	P	3077	0.06
132	1	I	3099	0.05
132	2	Q	3099	0.05
133	1	I	3077	0.04
133	2	R	3077	0.04
134	1	I	3057	0.07
134	2	S	3057	0.07
135	1	I	3100	0.05
135	2	T	3100	0.05
136	1	J	3131	0.05
136	2	K	3131	0.05
137	1	J	3476	0.07
137	2	L	3476	0.07
138	1	J	3484	0.06
138	2	M	3484	0.06
139	1	J	3391	0.08
139	2	N	3391	0.08
140	1	J	3479	0.06
140	2	O	3479	0.06
141	1	J	3503	0.06
141	2	P	3503	0.06
142	1	J	3162	0.04
142	2	Q	3162	0.04
143	1	J	3160	0.06
143	2	R	3160	0.06
144	1	J	3107	0.07
144	2	S	3107	0.07
145	1	J	3161	0.05
145	2	T	3161	0.05
146	1	K	3052	0.07
146	2	L	3052	0.07
147	1	K	3094	0.06
147	2	M	3094	0.06
148	1	K	3020	0.08
148	2	N	3020	0.08
149	1	K	3073	0.06
149	2	O	3073	0.06
150	1	K	3076	0.06
150	2	P	3076	0.06
151	1	K	3089	0.06
151	2	Q	3089	0.06
152	1	K	3062	0.06
152	2	R	3062	0.06
153	1	K	3050	0.07
153	2	S	3050	0.07
154	1	K	3084	0.07
154	2	T	3084	0.07
155	1	L	3387	0.08
155	2	M	3387	0.08
156	1	L	3350	0.08
156	2	N	3350	0.08
157	1	L	3393	0.08
157	2	O	3393	0.08
158	1	L	3431	0.08
158	2	P	3431	0.08
159	1	L	3079	0.07
159	2	Q	3079	0.07
160	1	L	3095	0.07
160	2	R	3095	0.07
161	1	L	3026	0.08
161	2	S	3026	0.08
162	1	L	3098	0.05
162	2	T	3098	0.05
163	1	M	3430	0.08
163	2	N	3430	0.08
164	1	M	3498	0.06
164	2	O	3498	0.06
165	1	M	3483	0.07
165	2	P	3483	0.07
166	1	M	3144	0.05
166	2	Q	3144	0.05
167	1	M	3147	0.06
167	2	R	3147	0.06
168	1	M	3110	0.06
168	2	S	3110	0.06
169	1	M	3141	0.06
169	2	T	3141	0.06
170	1	N	3351	0.08
170	2	O	3351	0.08
171	1	N	3348	0.09
171	2	P	3348	0.09
172	1	N	3014	0.07
172	2	Q	3014	0.07
173	1	N	3023	0.07
173	2	R	3023	0.07
174	1	N	2975	0.08
174	2	S	2975	0.08
175	1	N	3030	0.07
175	2	T	3030	0.07
176	1	O	3417	0.07
176	2	P	3417	0.07
177	1	O	3070	0.04
177	2	Q	3070	0.04
178	1	O	3069	0.06
178	2	R	3069	0.06
179	1	O	3044	0.07
179	2	S	3044	0.07
180	1	O	3065	0.06
180	2	T	3065	0.06
181	1	P	3115	0.05
181	2	Q	3115	0.05
182	1	P	3127	0.06
182	2	R	3127	0.06
183	1	P	3053	0.07
183	2	S	3053	0.07
184	1	P	3120	0.05
184	2	T	3120	0.05
185	1	Q	3104	0.03
185	2	R	3104	0.03
186	1	Q	3063	0.07
186	2	S	3063	0.07
187	1	Q	3121	0.05
187	2	T	3121	0.05
188	1	R	3053	0.07
188	2	S	3053	0.07
189	1	R	3104	0.04
189	2	T	3104	0.04
190	1	S	3183	0.07
190	2	T	3183	0.07

LS refinement shell

Resolution: 2.45→2.513 Å / Total num. of bins used: 20

	Rfactor	Num. reflection	% reflection
Rfree	0.289	505	-
Rwork	0.265	8856	-
obs	-	-	100 %

Refinement TLS params.

Method: refined / Refine-ID: X-RAY DIFFRACTION

ID	L11 (°2)	L12 (°2)	L13 (°2)	L22 (°2)	L23 (°2)	L33 (°2)	S11 (Å °)	S12 (Å °)	S13 (Å °)	S21 (Å °)	S22 (Å °)	S23 (Å °)	S31 (Å °)	S32 (Å °)	S33 (Å °)	T11 (Å2)	T12 (Å2)	T13 (Å2)	T22 (Å2)	T23 (Å2)	T33 (Å2)	Origin x (Å)	Origin y (Å)	Origin z (Å)
1	0.9515	0.4315	0.4383	2.2173	-0.5214	1.4728	0.0668	-0.0271	0.3791	0.1475	-0.2721	0.2899	-0.2027	0.0731	0.2052	0.2192	-0.0653	0.1178	0.1814	-0.267	0.9232	34.85	201.932	31.38
2	0.3248	0.3263	0.0338	1.4914	0.3371	1.8611	0.0248	-0.012	0.124	0.0542	-0.0219	0.4017	-0.0531	-0.0705	-0.0029	0.0185	0.0345	-0.0089	0.1503	-0.2787	0.8158	17.554	144.415	39.875
3	1.5636	-0.5649	0.0066	0.8809	-0.2492	2.5571	-0.1964	0.0389	-0.4152	-0.016	-0.2836	0.1838	0.2264	-0.2476	0.4801	0.0883	-0.0063	0.1493	0.1521	-0.1597	0.9564	39.509	102.326	78.459
4	1.7926	-0.1593	-0.1038	0.6363	-0.6489	1.2214	0.0933	0.2592	0.4471	-0.0351	-0.074	-0.1303	-0.0068	0.0432	-0.0193	0.0396	0.0049	0.0759	0.0457	0.0415	0.6019	96.532	82.749	86.713
5	9.8244	0.1076	-3.4991	0.1154	-0.1539	1.4076	-0.6048	0.5482	-0.4356	0.1171	-0.0593	-0.5409	0.2135	0.1443	0.6642	1.338	0.1246	-0.2962	1.9793	-0.1447	2.7322	50.813	160.938	33.834
6	0.1833	-0.0052	-0.8918	0.4039	-1.3047	9.9573	-0.1184	-0.2044	0.4327	0.0631	-0.0196	-0.7833	-0.5137	0.0849	0.1379	1.7064	-0.049	-0.0881	1.4905	-0.311	2.5639	49.496	135.528	70.47
7	7.6115	-0.5639	3.8362	7.7733	0.7355	2.147	0.6045	-0.128	0.738	-0.5191	-0.8964	-1.0633	-0.1524	-0.1518	0.2919	2.0169	-0.119	0.1457	1.4774	-0.0574	2.0367	72.604	119.94	84.781

Refinement TLS group

ID	Refine-ID	Refine TLS-ID	Auth asym-ID	Auth seq-ID
1	X-RAY DIFFRACTION	1	A	1 - 103
2	X-RAY DIFFRACTION	1	B	1 - 103
3	X-RAY DIFFRACTION	1	C	1 - 103
4	X-RAY DIFFRACTION	1	D	1 - 103
5	X-RAY DIFFRACTION	1	E	1 - 103
6	X-RAY DIFFRACTION	2	F	1 - 103
7	X-RAY DIFFRACTION	2	G	1 - 103
8	X-RAY DIFFRACTION	2	H	1 - 103
9	X-RAY DIFFRACTION	2	I	1 - 103
10	X-RAY DIFFRACTION	2	J	1 - 103
11	X-RAY DIFFRACTION	3	K	1 - 103
12	X-RAY DIFFRACTION	3	L	1 - 103
13	X-RAY DIFFRACTION	3	M	1 - 103
14	X-RAY DIFFRACTION	3	N	1 - 103
15	X-RAY DIFFRACTION	3	O	1 - 103
16	X-RAY DIFFRACTION	4	P	1 - 103
17	X-RAY DIFFRACTION	4	Q	1 - 103
18	X-RAY DIFFRACTION	4	R	1 - 103
19	X-RAY DIFFRACTION	4	S	1 - 103
20	X-RAY DIFFRACTION	4	T	1 - 103
21	X-RAY DIFFRACTION	5	E	104 - 124
22	X-RAY DIFFRACTION	5	F	104 - 124
23	X-RAY DIFFRACTION	5	G	104 - 124
24	X-RAY DIFFRACTION	6	J	104 - 124
25	X-RAY DIFFRACTION	6	L	104 - 124
26	X-RAY DIFFRACTION	6	M	104 - 124
27	X-RAY DIFFRACTION	7	N	104 - 124
28	X-RAY DIFFRACTION	7	O	104 - 124
29	X-RAY DIFFRACTION	7	P	104 - 124