PDB-6p6u: Crystal Structure of Monoclinic Rabbit Muscle Lactate Dehydrogena...

Basic information

• Entry: Database: PDB / ID: 6p6u
• Title: Crystal Structure of Monoclinic Rabbit Muscle Lactate Dehydrogenase with Four Tetramers as the Asymmetric Unit
• Components: L-lactate dehydrogenase A chain
• Keywords: OXIDOREDUCTASE / enzyme / AMP / NCS / isozyme / myosin

Function / homology

Function:

L-lactate dehydrogenase / lactate metabolic process / L-lactate dehydrogenase activity / pyruvate metabolic process / cytoplasm

Domain/homology:

L-lactate dehydrogenase / L-lactate dehydrogenase active site. / L-lactate dehydrogenase, active site / L-lactate/malate dehydrogenase / Lactate/malate dehydrogenase, N-terminal / Lactate/malate dehydrogenase, C-terminal / lactate/malate dehydrogenase, NAD binding domain / lactate/malate dehydrogenase, alpha/beta C-terminal domain / Lactate dehydrogenase/glycoside hydrolase, family 4, C-terminal / NAD(P)-binding domain superfamily

Component:

ADENOSINE MONOPHOSPHATE / L-lactate dehydrogenase A chain

• Biological species: Oryctolagus cuniculus (rabbit)
• Method: X-RAY DIFFRACTION / MOLECULAR REPLACEMENT / Resolution: 2.42 Å
• Authors: McPherson, A.
• Citation: Journal: to be published; Title: Crystal Structure of Monoclinic Rabbit Muscle Lactate Dehydrogenase with Four Tetramers as the Asymmetric Unit; Authors: McPherson, A.

History

Deposition	Jun 4, 2019	Deposition site: RCSB / Processing site: RCSB
Revision 1.0	Jun 17, 2020	Provider: repository / Type: Initial release
Revision 1.1	Oct 11, 2023	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: L-lactate dehydrogenase A chain

B: L-lactate dehydrogenase A chain

C: L-lactate dehydrogenase A chain

D: L-lactate dehydrogenase A chain

E: L-lactate dehydrogenase A chain

F: L-lactate dehydrogenase A chain

G: L-lactate dehydrogenase A chain

H: L-lactate dehydrogenase A chain

I: L-lactate dehydrogenase A chain

J: L-lactate dehydrogenase A chain

K: L-lactate dehydrogenase A chain

L: L-lactate dehydrogenase A chain

M: L-lactate dehydrogenase A chain

N: L-lactate dehydrogenase A chain

O: L-lactate dehydrogenase A chain

P: L-lactate dehydrogenase A chain

hetero molecules

Summary:

• 586 kDa, 16 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	586,496	18
Polymers	585,801	16
Non-polymers	694	2
Water	24,861	1380

1

A: L-lactate dehydrogenase A chain

B: L-lactate dehydrogenase A chain

C: L-lactate dehydrogenase A chain

D: L-lactate dehydrogenase A chain

hetero molecules

Summary:

• defined by author&software
• 147 kDa, 4 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	146,798	5
Polymers	146,450	4
Non-polymers	347	1
Water	72	4

Symmetry operations:

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

Calculated values:

Buried area	21590 Å2
ΔGint	-134 kcal/mol
Surface area	46610 Å2
Method	PISA

2

E: L-lactate dehydrogenase A chain

F: L-lactate dehydrogenase A chain

G: L-lactate dehydrogenase A chain

H: L-lactate dehydrogenase A chain

hetero molecules

Summary:

• defined by author&software
• 147 kDa, 4 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	146,798	5
Polymers	146,450	4
Non-polymers	347	1
Water	72	4

Symmetry operations:

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

Calculated values:

Buried area	21470 Å2
ΔGint	-132 kcal/mol
Surface area	46760 Å2
Method	PISA

3

I: L-lactate dehydrogenase A chain

J: L-lactate dehydrogenase A chain

K: L-lactate dehydrogenase A chain

L: L-lactate dehydrogenase A chain

Summary:

• defined by author&software
• 146 kDa, 4 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	146,450	4
Polymers	146,450	4
Non-polymers	0	0
Water	72	4

Symmetry operations:

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

Calculated values:

Buried area	21050 Å2
ΔGint	-141 kcal/mol
Surface area	46730 Å2
Method	PISA

4

M: L-lactate dehydrogenase A chain

N: L-lactate dehydrogenase A chain

O: L-lactate dehydrogenase A chain

P: L-lactate dehydrogenase A chain

Summary:

• defined by author&software
• 146 kDa, 4 polymers

Component details:

	Theoretical mass	Number of molelcules
Total (without water)	146,450	4
Polymers	146,450	4
Non-polymers	0	0
Water	72	4

Symmetry operations:

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

Calculated values:

Buried area	21150 Å2
ΔGint	-137 kcal/mol
Surface area	46710 Å2
Method	PISA

Unit cell

Length a, b, c (Å)	160.572, 100.838, 223.102
Angle α, β, γ (deg.)	90.00, 101.23, 90.00
Int Tables number	4
Space group name H-M	P1211

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	B
2	16	C
1	17	B
2	17	D
1	18	B
2	18	E
1	19	B
2	19	F
1	20	B
2	20	G
1	21	B
2	21	H
1	22	B
2	22	I
1	23	B
2	23	J
1	24	B
2	24	K
1	25	B
2	25	L
1	26	B
2	26	M
1	27	B
2	27	N
1	28	B
2	28	O
1	29	B
2	29	P
1	30	C
2	30	D
1	31	C
2	31	E
1	32	C
2	32	F
1	33	C
2	33	G
1	34	C
2	34	H
1	35	C
2	35	I
1	36	C
2	36	J
1	37	C
2	37	K
1	38	C
2	38	L
1	39	C
2	39	M
1	40	C
2	40	N
1	41	C
2	41	O
1	42	C
2	42	P
1	43	D
2	43	E
1	44	D
2	44	F
1	45	D
2	45	G
1	46	D
2	46	H
1	47	D
2	47	I
1	48	D
2	48	J
1	49	D
2	49	K
1	50	D
2	50	L
1	51	D
2	51	M
1	52	D
2	52	N
1	53	D
2	53	O
1	54	D
2	54	P
1	55	E
2	55	F
1	56	E
2	56	G
1	57	E
2	57	H
1	58	E
2	58	I
1	59	E
2	59	J
1	60	E
2	60	K
1	61	E
2	61	L
1	62	E
2	62	M
1	63	E
2	63	N
1	64	E
2	64	O
1	65	E
2	65	P
1	66	F
2	66	G
1	67	F
2	67	H
1	68	F
2	68	I
1	69	F
2	69	J
1	70	F
2	70	K
1	71	F
2	71	L
1	72	F
2	72	M
1	73	F
2	73	N
1	74	F
2	74	O
1	75	F
2	75	P
1	76	G
2	76	H
1	77	G
2	77	I
1	78	G
2	78	J
1	79	G
2	79	K
1	80	G
2	80	L
1	81	G
2	81	M
1	82	G
2	82	N
1	83	G
2	83	O
1	84	G
2	84	P
1	85	H
2	85	I
1	86	H
2	86	J
1	87	H
2	87	K
1	88	H
2	88	L
1	89	H
2	89	M
1	90	H
2	90	N
1	91	H
2	91	O
1	92	H
2	92	P
1	93	I
2	93	J
1	94	I
2	94	K
1	95	I
2	95	L
1	96	I
2	96	M
1	97	I
2	97	N
1	98	I
2	98	O
1	99	I
2	99	P
1	100	J
2	100	K
1	101	J
2	101	L
1	102	J
2	102	M
1	103	J
2	103	N
1	104	J
2	104	O
1	105	J
2	105	P
1	106	K
2	106	L
1	107	K
2	107	M
1	108	K
2	108	N
1	109	K
2	109	O
1	110	K
2	110	P
1	111	L
2	111	M
1	112	L
2	112	N
1	113	L
2	113	O
1	114	L
2	114	P
1	115	M
2	115	N
1	116	M
2	116	O
1	117	M
2	117	P
1	118	N
2	118	O
1	119	N
2	119	P
1	120	O
2	120	P

NCS domain segments:

Component-ID: _ / Beg auth comp-ID: ALA / Beg label comp-ID: ALA / End auth comp-ID: PHE / End label comp-ID: PHE / Refine code: _ / Auth seq-ID: 1 - 331 / Label seq-ID: 2 - 332

Dom-ID	Ens-ID	Auth asym-ID	Label asym-ID
1	1	A	A
2	1	B	B
1	2	A	A
2	2	C	C
1	3	A	A
2	3	D	D
1	4	A	A
2	4	E	E
1	5	A	A
2	5	F	F
1	6	A	A
2	6	G	G
1	7	A	A
2	7	H	H
1	8	A	A
2	8	I	I
1	9	A	A
2	9	J	J
1	10	A	A
2	10	K	K
1	11	A	A
2	11	L	L
1	12	A	A
2	12	M	M
1	13	A	A
2	13	N	N
1	14	A	A
2	14	O	O
1	15	A	A
2	15	P	P
1	16	B	B
2	16	C	C
1	17	B	B
2	17	D	D
1	18	B	B
2	18	E	E
1	19	B	B
2	19	F	F
1	20	B	B
2	20	G	G
1	21	B	B
2	21	H	H
1	22	B	B
2	22	I	I
1	23	B	B
2	23	J	J
1	24	B	B
2	24	K	K
1	25	B	B
2	25	L	L
1	26	B	B
2	26	M	M
1	27	B	B
2	27	N	N
1	28	B	B
2	28	O	O
1	29	B	B
2	29	P	P
1	30	C	C
2	30	D	D
1	31	C	C
2	31	E	E
1	32	C	C
2	32	F	F
1	33	C	C
2	33	G	G
1	34	C	C
2	34	H	H
1	35	C	C
2	35	I	I
1	36	C	C
2	36	J	J
1	37	C	C
2	37	K	K
1	38	C	C
2	38	L	L
1	39	C	C
2	39	M	M
1	40	C	C
2	40	N	N
1	41	C	C
2	41	O	O
1	42	C	C
2	42	P	P
1	43	D	D
2	43	E	E
1	44	D	D
2	44	F	F
1	45	D	D
2	45	G	G
1	46	D	D
2	46	H	H
1	47	D	D
2	47	I	I
1	48	D	D
2	48	J	J
1	49	D	D
2	49	K	K
1	50	D	D
2	50	L	L
1	51	D	D
2	51	M	M
1	52	D	D
2	52	N	N
1	53	D	D
2	53	O	O
1	54	D	D
2	54	P	P
1	55	E	E
2	55	F	F
1	56	E	E
2	56	G	G
1	57	E	E
2	57	H	H
1	58	E	E
2	58	I	I
1	59	E	E
2	59	J	J
1	60	E	E
2	60	K	K
1	61	E	E
2	61	L	L
1	62	E	E
2	62	M	M
1	63	E	E
2	63	N	N
1	64	E	E
2	64	O	O
1	65	E	E
2	65	P	P
1	66	F	F
2	66	G	G
1	67	F	F
2	67	H	H
1	68	F	F
2	68	I	I
1	69	F	F
2	69	J	J
1	70	F	F
2	70	K	K
1	71	F	F
2	71	L	L
1	72	F	F
2	72	M	M
1	73	F	F
2	73	N	N
1	74	F	F
2	74	O	O
1	75	F	F
2	75	P	P
1	76	G	G
2	76	H	H
1	77	G	G
2	77	I	I
1	78	G	G
2	78	J	J
1	79	G	G
2	79	K	K
1	80	G	G
2	80	L	L
1	81	G	G
2	81	M	M
1	82	G	G
2	82	N	N
1	83	G	G
2	83	O	O
1	84	G	G
2	84	P	P
1	85	H	H
2	85	I	I
1	86	H	H
2	86	J	J
1	87	H	H
2	87	K	K
1	88	H	H
2	88	L	L
1	89	H	H
2	89	M	M
1	90	H	H
2	90	N	N
1	91	H	H
2	91	O	O
1	92	H	H
2	92	P	P
1	93	I	I
2	93	J	J
1	94	I	I
2	94	K	K
1	95	I	I
2	95	L	L
1	96	I	I
2	96	M	M
1	97	I	I
2	97	N	N
1	98	I	I
2	98	O	O
1	99	I	I
2	99	P	P
1	100	J	J
2	100	K	K
1	101	J	J
2	101	L	L
1	102	J	J
2	102	M	M
1	103	J	J
2	103	N	N
1	104	J	J
2	104	O	O
1	105	J	J
2	105	P	P
1	106	K	K
2	106	L	L
1	107	K	K
2	107	M	M
1	108	K	K
2	108	N	N
1	109	K	K
2	109	O	O
1	110	K	K
2	110	P	P
1	111	L	L
2	111	M	M
1	112	L	L
2	112	N	N
1	113	L	L
2	113	O	O
1	114	L	L
2	114	P	P
1	115	M	M
2	115	N	N
1	116	M	M
2	116	O	O
1	117	M	M
2	117	P	P
1	118	N	N
2	118	O	O
1	119	N	N
2	119	P	P
1	120	O	O
2	120	P	P

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

Components

#1: Protein

A B C D E F G H I J K L M N O P
L-lactate dehydrogenase A chain / LDH-A / LDH muscle subunit / LDH-M

Details:

Mass: 36612.574 Da / Num. of mol.: 16
Source method: isolated from a genetically manipulated source
Source: (gene. exp.) Oryctolagus cuniculus (rabbit) / Gene: LDHA / Production host: Oryctolagus cuniculus (rabbit) / References: UniProt: P13491, L-lactate dehydrogenase

#2: Chemical

C-401 E-401 ChemComp-AMP / ADENOSINE MONOPHOSPHATE

Details:

Mass: 347.221 Da / Num. of mol.: 2 / Source method: obtained synthetically / Formula: C₁₀H₁₄N₅O₇P / Comment: AMP*YM

#3: Water

ChemComp-HOH / water

Details:

Mass: 18.015 Da / Num. of mol.: 1380 / 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: 3.04 ų/Da / Density % sol: 59.5 % / Description: thick blocks
• Crystal grow: Temperature: 298 K / Method: vapor diffusion, sitting drop / pH: 7 ; Details: Sitting drop composed of equal amounts of 20% PEG 3350 in .10 M Tris buffer pH 7.0 and a 30 mg/ml stock protein solution containing 0.1 M Tris pH 7.0. Reservoir 20% PEG 3350 in water.; PH range: 6.5 - 7.5

Data collection

• Diffraction: Mean temperature: 298 K / Serial crystal experiment: N
• Diffraction source: Source: ROTATING ANODE / Type: RIGAKU RU200 / Wavelength: 1.54 Å
• Detector: Type: SDMS / Detector: AREA DETECTOR / Date: Sep 15, 1995 / Details: bent crystal monochromator
• Radiation: Protocol: SINGLE WAVELENGTH / Monochromatic (M) / Laue (L): M / Scattering type: x-ray
• Radiation wavelength: Wavelength: 1.54 Å / Relative weight: 1
• Reflection: Resolution: 2.4→60 Å / % possible obs: 88 % / Observed criterion σ(F): 3 / Redundancy: 6.5 % / B_iso Wilson estimate: 52 Ų / CC_1/2: 0.97 / R_merge(I) obs: 0.13 / R_sym value: 0.12 / Net I/σ(I): 7.4
• Reflection shell: Resolution: 2.4→2.45 Å / Redundancy: 3 % / R_merge(I) obs: 0.28 / Mean I/σ(I) obs: 3.3 / Num. unique obs: 3000 / CC_1/2: 0.54 / R_rim(I) all: 0.28 / % possible all: 22

Processing

Software

Name	Version	Classification
REFMAC	5.8.0155	refinement
DENZO		data reduction
SCALEPACK		data scaling
PHASER		phasing

Refinement

Method to determine structure: MOLECULAR REPLACEMENT
Starting model: 6LDH

6ldh

Resolution: 2.42→60 Å / Cor.coef. F_o:F_c: 0.966 / Cor.coef. F_o:F_c free: 0.957 / SU B: 27.162 / SU ML: 0.277 / Cross valid method: THROUGHOUT / ESU R Free: 0.392 / Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS

	Rfactor	Num. reflection	% reflection	Selection details
Rfree	0.21338	13675	10 %	RANDOM
Rwork	0.18092	-	-	-
obs	0.18412	123133	51.51 %	-

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

Displacement parameters

B_iso mean: 52.132 Ų

	Baniso -1	Baniso -2	Baniso -3
1-	-1.27 Å2	0 Å2	1.69 Å2
2-	-	2.47 Å2	0 Å2
3-	-	-	-1.73 Å2

Refinement step

Cycle: 1 / Resolution: 2.42→60 Å

	Protein	Nucleic acid	Ligand	Solvent	Total
Num. atoms	40944	0	46	1380	42370

Refine LS restraints

Refine-ID	Type	Dev ideal	Dev ideal target	Number
X-RAY DIFFRACTION	r_bond_refined_d	0.009	0.019	41843
X-RAY DIFFRACTION	r_bond_other_d	0.001	0.02	41760
X-RAY DIFFRACTION	r_angle_refined_deg	1.281	1.965	56635
X-RAY DIFFRACTION	r_angle_other_deg	0.67	3	96206
X-RAY DIFFRACTION	r_dihedral_angle_1_deg	5.174	5	5312
X-RAY DIFFRACTION	r_dihedral_angle_2_deg	36.79	24.929	1627
X-RAY DIFFRACTION	r_dihedral_angle_3_deg	15.106	15	7746
X-RAY DIFFRACTION	r_dihedral_angle_4_deg	24.182	15	164
X-RAY DIFFRACTION	r_chiral_restr	0.081	0.2	6634
X-RAY DIFFRACTION	r_gen_planes_refined	0.005	0.02	46448
X-RAY DIFFRACTION	r_gen_planes_other	0.001	0.02	8900
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	3.041	3.671	21200
X-RAY DIFFRACTION	r_mcbond_other	3.04	3.67	21199
X-RAY DIFFRACTION	r_mcangle_it	4.954	5.502	26480
X-RAY DIFFRACTION	r_mcangle_other	4.954	5.502	26481
X-RAY DIFFRACTION	r_scbond_it	3.908	4.312	20643
X-RAY DIFFRACTION	r_scbond_other	3.908	4.312	20644
X-RAY DIFFRACTION	r_scangle_it
X-RAY DIFFRACTION	r_scangle_other	6.459	6.24	30140
X-RAY DIFFRACTION	r_long_range_B_refined	9.963	70.436	171517
X-RAY DIFFRACTION	r_long_range_B_other	9.963	70.436	171518
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	20338	0.09
1	2	B	20338	0.09
2	1	A	20206	0.1
2	2	C	20206	0.1
3	1	A	20154	0.1
3	2	D	20154	0.1
4	1	A	20070	0.11
4	2	E	20070	0.11
5	1	A	20146	0.1
5	2	F	20146	0.1
6	1	A	20274	0.1
6	2	G	20274	0.1
7	1	A	20226	0.1
7	2	H	20226	0.1
8	1	A	20064	0.11
8	2	I	20064	0.11
9	1	A	20106	0.1
9	2	J	20106	0.1
10	1	A	20002	0.1
10	2	K	20002	0.1
11	1	A	20152	0.1
11	2	L	20152	0.1
12	1	A	20216	0.1
12	2	M	20216	0.1
13	1	A	20188	0.1
13	2	N	20188	0.1
14	1	A	19978	0.12
14	2	O	19978	0.12
15	1	A	20166	0.1
15	2	P	20166	0.1
16	1	B	20270	0.1
16	2	C	20270	0.1
17	1	B	20166	0.1
17	2	D	20166	0.1
18	1	B	20014	0.11
18	2	E	20014	0.11
19	1	B	20232	0.1
19	2	F	20232	0.1
20	1	B	20232	0.09
20	2	G	20232	0.09
21	1	B	20158	0.1
21	2	H	20158	0.1
22	1	B	20128	0.1
22	2	I	20128	0.1
23	1	B	20194	0.1
23	2	J	20194	0.1
24	1	B	20054	0.1
24	2	K	20054	0.1
25	1	B	20070	0.1
25	2	L	20070	0.1
26	1	B	20298	0.09
26	2	M	20298	0.09
27	1	B	20234	0.1
27	2	N	20234	0.1
28	1	B	20092	0.11
28	2	O	20092	0.11
29	1	B	20280	0.1
29	2	P	20280	0.1
30	1	C	20286	0.1
30	2	D	20286	0.1
31	1	C	20150	0.11
31	2	E	20150	0.11
32	1	C	20200	0.11
32	2	F	20200	0.11
33	1	C	20384	0.1
33	2	G	20384	0.1
34	1	C	20288	0.1
34	2	H	20288	0.1
35	1	C	20106	0.11
35	2	I	20106	0.11
36	1	C	20060	0.11
36	2	J	20060	0.11
37	1	C	20092	0.11
37	2	K	20092	0.11
38	1	C	20254	0.11
38	2	L	20254	0.11
39	1	C	20230	0.1
39	2	M	20230	0.1
40	1	C	20172	0.12
40	2	N	20172	0.12
41	1	C	20008	0.12
41	2	O	20008	0.12
42	1	C	20346	0.1
42	2	P	20346	0.1
43	1	D	20090	0.1
43	2	E	20090	0.1
44	1	D	20194	0.1
44	2	F	20194	0.1
45	1	D	20282	0.1
45	2	G	20282	0.1
46	1	D	20414	0.09
46	2	H	20414	0.09
47	1	D	20054	0.11
47	2	I	20054	0.11
48	1	D	20176	0.1
48	2	J	20176	0.1
49	1	D	20076	0.1
49	2	K	20076	0.1
50	1	D	20474	0.09
50	2	L	20474	0.09
51	1	D	20122	0.1
51	2	M	20122	0.1
52	1	D	20216	0.1
52	2	N	20216	0.1
53	1	D	20084	0.11
53	2	O	20084	0.11
54	1	D	20330	0.1
54	2	P	20330	0.1
55	1	E	20226	0.1
55	2	F	20226	0.1
56	1	E	20168	0.11
56	2	G	20168	0.11
57	1	E	20186	0.11
57	2	H	20186	0.11
58	1	E	19982	0.11
58	2	I	19982	0.11
59	1	E	20074	0.11
59	2	J	20074	0.11
60	1	E	20090	0.11
60	2	K	20090	0.11
61	1	E	20028	0.11
61	2	L	20028	0.11
62	1	E	20174	0.11
62	2	M	20174	0.11
63	1	E	20218	0.11
63	2	N	20218	0.11
64	1	E	20064	0.12
64	2	O	20064	0.12
65	1	E	20218	0.11
65	2	P	20218	0.11
66	1	F	20368	0.1
66	2	G	20368	0.1
67	1	F	20278	0.11
67	2	H	20278	0.11
68	1	F	20140	0.11
68	2	I	20140	0.11
69	1	F	20106	0.11
69	2	J	20106	0.11
70	1	F	20162	0.11
70	2	K	20162	0.11
71	1	F	20116	0.11
71	2	L	20116	0.11
72	1	F	20206	0.11
72	2	M	20206	0.11
73	1	F	20274	0.1
73	2	N	20274	0.1
74	1	F	20042	0.12
74	2	O	20042	0.12
75	1	F	20276	0.1
75	2	P	20276	0.1
76	1	G	20504	0.09
76	2	H	20504	0.09
77	1	G	20224	0.11
77	2	I	20224	0.11
78	1	G	20114	0.11
78	2	J	20114	0.11
79	1	G	20168	0.11
79	2	K	20168	0.11
80	1	G	20252	0.1
80	2	L	20252	0.1
81	1	G	20230	0.1
81	2	M	20230	0.1
82	1	G	20288	0.1
82	2	N	20288	0.1
83	1	G	20100	0.12
83	2	O	20100	0.12
84	1	G	20374	0.1
84	2	P	20374	0.1
85	1	H	20252	0.1
85	2	I	20252	0.1
86	1	H	20140	0.11
86	2	J	20140	0.11
87	1	H	20216	0.1
87	2	K	20216	0.1
88	1	H	20490	0.09
88	2	L	20490	0.09
89	1	H	20142	0.11
89	2	M	20142	0.11
90	1	H	20354	0.1
90	2	N	20354	0.1
91	1	H	20012	0.12
91	2	O	20012	0.12
92	1	H	20384	0.1
92	2	P	20384	0.1
93	1	I	20014	0.12
93	2	J	20014	0.12
94	1	I	19868	0.12
94	2	K	19868	0.12
95	1	I	20028	0.11
95	2	L	20028	0.11
96	1	I	20146	0.11
96	2	M	20146	0.11
97	1	I	20102	0.11
97	2	N	20102	0.11
98	1	I	19910	0.13
98	2	O	19910	0.13
99	1	I	20146	0.11
99	2	P	20146	0.11
100	1	J	19868	0.12
100	2	K	19868	0.12
101	1	J	20196	0.11
101	2	L	20196	0.11
102	1	J	20148	0.11
102	2	M	20148	0.11
103	1	J	20304	0.1
103	2	N	20304	0.1
104	1	J	20154	0.11
104	2	O	20154	0.11
105	1	J	20170	0.11
105	2	P	20170	0.11
106	1	K	20084	0.11
106	2	L	20084	0.11
107	1	K	20120	0.11
107	2	M	20120	0.11
108	1	K	20114	0.11
108	2	N	20114	0.11
109	1	K	20078	0.12
109	2	O	20078	0.12
110	1	K	20128	0.11
110	2	P	20128	0.11
111	1	L	20166	0.11
111	2	M	20166	0.11
112	1	L	20302	0.1
112	2	N	20302	0.1
113	1	L	20032	0.12
113	2	O	20032	0.12
114	1	L	20348	0.1
114	2	P	20348	0.1
115	1	M	20210	0.11
115	2	N	20210	0.11
116	1	M	20030	0.12
116	2	O	20030	0.12
117	1	M	20288	0.11
117	2	P	20288	0.11
118	1	N	20096	0.12
118	2	O	20096	0.12
119	1	N	20324	0.1
119	2	P	20324	0.1
120	1	O	20198	0.11
120	2	P	20198	0.11

LS refinement shell

Resolution: 2.423→2.486 Å / Total num. of bins used: 20

	Rfactor	Num. reflection	% reflection
Rfree	0.357	65	-
Rwork	0.327	541	-
obs	-	-	3.1 %

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	0.215	-0.041	-0.0544	0.3441	0.0323	0.3443	-0.0015	0.0157	0.1581	0.0147	-0.0454	0.0473	-0.0559	-0.0336	0.0469	0.0942	0.0183	-0.0997	0.0416	-0.0203	0.2414	28.8451	27.0206	100.5794
2	0.1641	-0.0581	-0.1217	0.3155	0.0838	0.408	-0.0437	0.1446	-0.0353	0.0155	-0.0241	-0.0007	0.023	-0.026	0.0678	0.0763	-0.0186	-0.0499	0.1581	-0.0477	0.0949	33.7533	-5.4694	82.4918
3	0.4531	-0.1592	0.1098	0.1602	-0.0986	0.1134	-0.0754	-0.027	0.0103	0.042	0.0406	-0.0358	0.0266	0.0312	0.0348	0.1426	0.073	-0.0825	0.0779	-0.0095	0.1239	48.4969	-5.426	112.5159
4	0.3952	-0.0729	-0.2163	0.0666	-0.0042	0.39	-0.1125	-0.026	0.0278	0.0266	-0.0145	0.0396	0.033	-0.0431	0.127	0.0908	0.0095	-0.0293	0.0893	-0.0793	0.1715	11.7526	1.8002	114.8451
5	0.3369	0.0652	-0.067	0.2679	0.1573	0.5091	-0.0064	0.0119	0.1773	-0.0093	-0.0094	-0.0466	-0.0313	0.0059	0.0158	0.0845	-0.0096	-0.0959	0.0253	0.0256	0.2372	29.7263	27.0273	8.7949
6	0.2009	-0.0321	-0.0346	0.2412	-0.0461	0.4145	-0.0438	-0.1398	-0.0416	-0.003	-0.016	-0.0258	0.0296	-0.0085	0.0598	0.0702	0.0082	-0.0462	0.1419	0.0553	0.1136	24.7961	-5.4813	26.9416
7	0.4056	0.1332	-0.0206	0.2722	0.0679	0.1503	-0.0861	0.0147	-0.0279	-0.0428	0.063	0.0316	0.0304	-0.0477	0.0231	0.0912	-0.0399	-0.0763	0.0752	0.0128	0.1539	10.0586	-5.414	-3.1089
8	0.5396	0.2263	-0.1939	0.1498	0.0226	0.4822	-0.1234	0.0113	-0.0152	-0.0402	-0.0184	-0.0301	0.0239	0.0529	0.1418	0.0721	-0.0005	-0.0402	0.0885	0.0958	0.1607	46.8019	1.8194	-5.4209
9	0.4191	0.0097	-0.3551	0.4256	0.0407	0.3824	0.0771	0.1879	0.1894	0.039	0.0798	-0.1244	-0.0082	-0.0946	-0.1569	0.0701	0.0652	0.0034	0.1432	0.0879	0.1639	76.7802	95.3234	29.1847
10	0.4398	-0.1671	-0.4761	0.0938	0.1551	0.6056	-0.072	-0.2359	0.086	0.0301	0.1395	0.0006	0.0367	0.1494	-0.0675	0.0724	0.1122	-0.0549	0.2518	-0.0517	0.0748	71.0862	87.1761	65.4242
11	0.56	-0.2432	-0.2788	0.5131	0.0242	0.2928	-0.2208	0.0591	-0.0593	0.0678	0.1321	0	0.1003	-0.1633	0.0887	0.1027	-0.0127	0.0289	0.1682	-0.0078	0.0868	55.6742	65.5353	45.0205
12	0.5742	-0.1377	-0.3243	0.0798	0.1325	0.3073	-0.1642	-0.0409	0.0292	0.0443	0.0823	0.0202	0.1525	0.1326	0.0819	0.1355	0.1036	0.0091	0.1866	0.026	0.0895	92.6624	67.2393	38.5585
13	0.478	0.0404	-0.4172	0.0162	-0.0472	0.4908	0.1343	-0.1843	0.1938	-0.0204	0.0035	0.0489	-0.0362	0.0889	-0.1378	0.1144	-0.0758	-0.0143	0.1132	-0.0945	0.1798	-18.1855	95.3071	80.2237
14	0.3622	0.1825	-0.471	0.2092	-0.178	0.7195	-0.074	0.2232	0.1013	0.0056	0.1907	-0.0272	0.0766	-0.1761	-0.1167	0.1023	-0.1002	-0.0924	0.2594	0.0622	0.0995	-12.4836	87.1779	43.9897
15	0.5269	0.2787	-0.2364	0.3437	-0.0215	0.3441	-0.2093	-0.0441	-0.0634	-0.0729	0.1008	-0.0161	0.1039	0.1689	0.1085	0.132	0.0151	0.0373	0.1545	0.0055	0.0865	2.8898	65.5266	64.3999
16	0.6184	0.0795	-0.3974	0.2325	-0.2621	0.4594	-0.2141	0.0849	0.0086	0.0094	0.1183	-0.0997	0.124	-0.1684	0.0958	0.1633	-0.1081	-0.0374	0.1722	-0.0218	0.0502	-34.0825	67.2646	70.865

Refinement TLS group

ID	Refine-ID	Refine TLS-ID	Auth asym-ID	Auth seq-ID
1	X-RAY DIFFRACTION	1	A	1 - 331
2	X-RAY DIFFRACTION	2	B	1 - 331
3	X-RAY DIFFRACTION	3	C	1 - 331
4	X-RAY DIFFRACTION	4	D	1 - 331
5	X-RAY DIFFRACTION	5	E	1 - 331
6	X-RAY DIFFRACTION	6	F	1 - 331
7	X-RAY DIFFRACTION	7	G	1 - 331
8	X-RAY DIFFRACTION	8	H	1 - 331
9	X-RAY DIFFRACTION	9	I	1 - 331
10	X-RAY DIFFRACTION	10	J	1 - 331
11	X-RAY DIFFRACTION	11	K	1 - 331
12	X-RAY DIFFRACTION	12	L	1 - 331
13	X-RAY DIFFRACTION	13	M	1 - 331
14	X-RAY DIFFRACTION	14	N	1 - 331
15	X-RAY DIFFRACTION	15	O	1 - 331
16	X-RAY DIFFRACTION	16	P	1 - 331