PDB-4m1u: The crystal structure of Stx2 and a disaccharide ligand

ID or keywords:

Entry

Database: PDB / ID: 4m1u

Title

The crystal structure of Stx2 and a disaccharide ligand

Components

Shiga toxin 2 A-subunit
Shiga toxin 2 B subunit

Keywords

HYDROLASE /

rRNA N-glycosylase

Function / homology

Function and homology information

hemolysis by symbiont of host erythrocytes /

rRNA N-glycosylase /

rRNA N-glycosylase activity /

toxin activity / negative regulation of translation / extracellular region
Similarity search - Function

Biological species

Escherichia coli O157:H7 (bacteria)

Escherichia coli (E. coli)

Method

X-RAY DIFFRACTION /

SYNCHROTRON /

MOLECULAR REPLACEMENT / Resolution: 1.56 Å

Authors

Yin, J. / James, M.N.G. / Jacobson, J.M. / Kitov, P.I. / Bundle, D.R. / Mulvey, G. / Armstrong, G.

Citation

Journal: J.Biol.Chem. / Year: 2014
Title: The crystal structure of shiga toxin type 2 with bound disaccharide guides the design of a heterobifunctional toxin inhibitor.
Authors: Jacobson, J.M. / Yin, J. / Kitov, P.I. / Mulvey, G. / Griener, T.P. / James, M.N. / Armstrong, G. / Bundle, D.R.

History

Deposition	Aug 4, 2013	Deposition site: RCSB / Processing site: RCSB
Revision 1.0	Nov 20, 2013	Provider: repository / Type: Initial release
Revision 1.1	Dec 4, 2013	Group: Database references
Revision 1.2	Feb 19, 2014	Group: Database references
Revision 2.0	Jul 29, 2020	Group: Atomic model / Data collection ...Atomic model / Data collection / Derived calculations / Structure summary Category: atom_site / chem_comp ...atom_site / chem_comp / entity / pdbx_branch_scheme / pdbx_chem_comp_identifier / pdbx_entity_branch / pdbx_entity_branch_descriptor / pdbx_entity_branch_link / pdbx_entity_branch_list / pdbx_entity_nonpoly / pdbx_nonpoly_scheme / pdbx_struct_assembly_gen / struct_asym / struct_conn / struct_site / struct_site_gen Item: _atom_site.B_iso_or_equiv / _atom_site.Cartn_x ..._atom_site.B_iso_or_equiv / _atom_site.Cartn_x / _atom_site.Cartn_y / _atom_site.Cartn_z / _atom_site.auth_asym_id / _atom_site.auth_atom_id / _atom_site.auth_comp_id / _atom_site.auth_seq_id / _atom_site.label_asym_id / _atom_site.label_atom_id / _atom_site.label_comp_id / _atom_site.label_entity_id / _atom_site.type_symbol / _chem_comp.mon_nstd_flag / _chem_comp.name / _chem_comp.pdbx_synonyms / _chem_comp.type / _pdbx_struct_assembly_gen.asym_id_list / _struct_conn.pdbx_leaving_atom_flag / _struct_conn.ptnr1_auth_asym_id / _struct_conn.ptnr1_auth_comp_id / _struct_conn.ptnr1_auth_seq_id / _struct_conn.ptnr1_label_asym_id / _struct_conn.ptnr1_label_atom_id / _struct_conn.ptnr1_label_comp_id / _struct_conn.ptnr2_auth_asym_id / _struct_conn.ptnr2_auth_comp_id / _struct_conn.ptnr2_auth_seq_id / _struct_conn.ptnr2_label_asym_id / _struct_conn.ptnr2_label_atom_id / _struct_conn.ptnr2_label_comp_id Description: Carbohydrate remediation / Provider: repository / Type: Remediation
Revision 2.1	Sep 20, 2023	Group: Data collection / Database references ...Data collection / Database references / Refinement description / Structure summary Category: chem_comp / chem_comp_atom ...chem_comp / chem_comp_atom / chem_comp_bond / database_2 / pdbx_initial_refinement_model Item: _chem_comp.pdbx_synonyms / _database_2.pdbx_DOI / _database_2.pdbx_database_accession

Structure viewer	Molecule: MolmilJmol/JSmol

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Download

PDBx/mmCIF format	4m1u.cif.gz	273.7 KB	Display	PDBx/mmCIF format
PDB format	pdb4m1u.ent.gz	222.6 KB	Display	PDB format
PDBx/mmJSON format	4m1u.json.gz		Tree view	PDBx/mmJSON format
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Validation report

Arichive directory	https://data.pdbj.org/pub/pdb/validation_reports/m1/4m1u ftp://data.pdbj.org/pub/pdb/validation_reports/m1/4m1u	HTTPS FTP

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Related structure data

Related structure data	1r4pS 1bos S: Starting model for refinement
Similar structure data	6u3u-2 7d6r-d 5yb0-2 7d6q-d 7a9i-d 2bi2-d 2ww3-3 2wzs-4 2xsg-1 3fd6-d Search similar-shape structures by Omokage search (details) Similarity search - Function & homologyF&H Search Similarity search - FunctionF&H Search Similarity search - HomologyF&H Search

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Links

PDB pages	PDBj / wwPDB / NCBI
Related items in Molecule of the Month	#161 - May 2013 Ricin similarity (8) #69 - Sep 2005 Cholera Toxin similarity (9)

Deposited unit

A: Shiga toxin 2 A-subunit

B: Shiga toxin 2 B subunit

C: Shiga toxin 2 B subunit

D: Shiga toxin 2 B subunit

E: Shiga toxin 2 B subunit

F: Shiga toxin 2 B subunit

hetero molecules

73.7 kDa, 6 polymers
Search similar-shape structures of this assembly by Omokage search (details)

1

Idetical with deposited unit
defined by author&software

Unit cell

Length a, b, c (Å)	146.250, 146.250, 60.310
Angle α, β, γ (deg.)	90.00, 90.00, 120.00
Int Tables number	169
Space group name H-M	P6₁

#1: Protein

Shiga toxin 2 A-subunit / Shiga toxin 2 subunit A / Shiga-like toxin II A subunit encoded by bacteriophage BP-933W

Mass: 33228.215 Da / Num. of mol.: 1 / Fragment: Stx2 subunit A (unp entries 230-319)
Source method: isolated from a genetically manipulated source
Source: (gene. exp.)

Escherichia coli O157:H7 (bacteria)
Gene: ECs1205, stx 2 A-subunit, stx2 A-subunit, stx2A, Z1464
Production host:

Escherichia coli (E. coli) / References: UniProt: Q7DI68,

rRNA N-glycosylase

#2: Protein

Shiga toxin 2 B subunit / Shiga toxin 2 subunit B / Shiga toxin 2 / subunit B / Shiga toxin 2v subunit A / Shiga toxin 2v ...

Mass: 7824.590 Da / Num. of mol.: 5 / Fragment: Stx2 subunit B (unp entries 20-89)
Source method: isolated from a genetically manipulated source
Source: (gene. exp.)

Escherichia coli (E. coli) / Gene: stx2B, stx2dB, stx2vB, stxB2, stxII, vtx2B / Production host:

Escherichia coli (E. coli) / References: UniProt: Q7DJJ2

#3: Polysaccharide

2-acetamido-2-deoxy-alpha-D-galactopyranose-(1-4)-methyl beta-D-galactopyranoside

Type: oligosaccharide

/ Mass: 397.375 Da / Num. of mol.: 2
Source method: isolated from a genetically manipulated source

Descriptor	Type	Program
DGalpNAca1-4DGalp[1Me]b1-OME	Glycam Condensed Sequence	GMML 1.0
WURCS=2.0/2,2,1/[a2112h-1b_1-5_1OC][a2112h-1a_1-5_2NCC/3=O]/1-2/a4-b1	WURCS	PDB2Glycan 1.1.0
[][methyl]{[(1+1)][b-D-Galp]{[(4+1)][a-D-GalpNAc]{}}}	LINUCS	PDB-CARE

#4: Chemical

ChemComp-1PS / 3-PYRIDINIUM-1-YLPROPANE-1-SULFONATE / 1-(3-SULFOPROPYL) PYRIDINIUM / PPS

Mass: 201.243 Da / Num. of mol.: 3 / Source method: obtained synthetically / Formula: C₈H₁₁NO₃S

#5: Water

ChemComp-HOH / water /

Water

Mass: 18.015 Da / Num. of mol.: 732 / Source method: isolated from a natural source / Formula: H₂O

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Experiment

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

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Sample preparation

Crystal	Density Matthews: 2.57 Å³/Da / Density % sol: 52.2 %
Crystal grow	Temperature: 297 K / Method: vapor diffusion, hanging drop / pH: 7 Details: 3.8 M sodium formate, 50 mM Tris pH 7.0, 2% ethylene glycol, and 1 mM PPS (3-(1-pyridino)-1-propanesulfonate) , VAPOR DIFFUSION, HANGING DROP, temperature 297K

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Data collection

Diffraction	Mean temperature: 100 K
Diffraction source	Source: SYNCHROTRON / Site: CLSI / Beamline: 08B1-1 / Wavelength: 0.97949 Å
Detector	Type: MAR scanner 300 mm plate / Detector: IMAGE PLATE / Date: Jul 1, 2012
Radiation	Monochromator: DCM, Si(111) Watercooled first crystal / Protocol: SINGLE WAVELENGTH / Monochromatic (M) / Laue (L): M / Scattering type: x-ray
Radiation wavelength	Wavelength: 0.97949 Å / Relative weight: 1
Reflection	Resolution: 1.56→50 Å / Num. all: 206175 / Num. obs: 104677 / % possible obs: 92.8 % / Observed criterion σ(F): 0 / Observed criterion σ(I): -3 / R_sym value: 0.082 / Net I/σ(I): 8.8
Reflection shell	Resolution: 1.56→1.65 Å / Redundancy: 2.9 % / Mean I/σ(I) obs: 1.4 / Num. unique all: 29975 / R_sym value: 0.978 / % possible all: 89.9

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Processing

Software

Name	Version	Classification
MxDC		data collection
PHASER		phasing
REFMAC	5.5.0055	refinement
XDS		data reduction
XDS		data scaling

Refinement

Method to determine structure:

MOLECULAR REPLACEMENT
Starting model: pdb entry 1R4P

1r4p

Resolution: 1.56→40 Å / Cor.coef. F_o:F_c: 0.972 / Cor.coef. F_o:F_c free: 0.963 / SU B: 3.301 / SU ML: 0.052 / Cross valid method: THROUGHOUT / σ(F): 0 / ESU R: 0.075 / ESU R Free: 0.074 / Stereochemistry target values: MAXIMUM LIKELIHOOD / Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS

	R_factor	Num. reflection	% reflection	Selection details
R_free	0.19193	5229	5 %	RANDOM
R_work	0.17031	-	-	-
obs	0.1714	99444	99.59 %	-
all	-	99853	-	-

Solvent computation

Ion probe radii: 0.8 Å / Shrinkage radii: 0.8 Å / VDW probe radii: 1.2 Å / Solvent model: MASK

Displacement parameters

B_iso mean: 25.06 Å²

	B_aniso -1	B_aniso -2	B_aniso -3
1-	-0.17 Å²	-0.09 Å²	0 Å²
2-	-	-0.17 Å²	0 Å²
3-	-	-	0.26 Å²

Refinement step

Cycle: LAST / Resolution: 1.56→40 Å

	Protein	Nucleic acid	Ligand	Solvent	Total
Num. atoms	4961	0	93	732	5786

Refine LS restraints

Refine-ID	Type	Dev ideal	Dev ideal target	Number
X-RAY DIFFRACTION	r_bond_refined_d	0.006	0.022	5163
X-RAY DIFFRACTION	r_angle_refined_deg	0.989	1.952	6999
X-RAY DIFFRACTION	r_dihedral_angle_1_deg	5.336	5	624
X-RAY DIFFRACTION	r_dihedral_angle_2_deg	32.566	24.752	242
X-RAY DIFFRACTION	r_dihedral_angle_3_deg	11.644	15	861
X-RAY DIFFRACTION	r_dihedral_angle_4_deg	15.039	15	27
X-RAY DIFFRACTION	r_chiral_restr	0.069	0.2	797
X-RAY DIFFRACTION	r_gen_planes_refined	0.004	0.02	3867
X-RAY DIFFRACTION	r_mcbond_it	0.32	1.5	3127
X-RAY DIFFRACTION	r_mcangle_it	0.619	2	5068
X-RAY DIFFRACTION	r_scbond_it	0.943	3	2036
X-RAY DIFFRACTION	r_scangle_it	1.512	4.5	1931

LS refinement shell

Resolution: 1.558→1.598 Å / Total num. of bins used: 20

	R_factor	Num. reflection	% reflection
R_free	0.315	386	-
R_work	0.318	7149	-
obs	-	-	97.45 %

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	2.3598	-1.5245	0.0548	4.5983	1.2995	3.0824	-0.0578	-0.0473	0.2527	0.1718	0.026	-0.1239	-0.2083	0.0188	0.0319	0.1002	-0.0056	0.0145	0.119	0.0084	0.1031	17.1708	63.8006	-10.9431
2	0.7293	-0.1352	-0.1264	0.5519	-0.3583	1.0169	-0.0088	-0.0215	0.081	0.0218	-0.0204	0.0026	-0.1024	0.0414	0.0291	0.1081	-0.003	-0.0013	0.1334	-0.0022	0.133	13.5179	63.7392	-2.2833
3	1.7021	-0.6282	0.5124	1.3303	0.0885	1.3004	-0.0287	0.0935	0.2076	0.0071	-0.0371	-0.0966	-0.0462	-0.0002	0.0658	0.0738	0.0079	-0.0113	0.0961	0.0317	0.132	6.9406	73.5667	-13.3197
4	1.4631	-0.6331	0.0473	1.3547	-0.3848	0.6605	-0.0151	0.0835	0.1368	0.0044	0.0196	0.0372	-0.0207	-0.0667	-0.0045	0.0746	0.0045	-0.0193	0.1286	0.013	0.0767	-0.9736	68.9234	-17.0744
5	0.4508	-0.4436	0.2382	0.7529	-0.329	1.2739	0.0047	0.0324	-0.022	-0.0483	0.0442	0.007	0.0487	-0.0361	-0.0489	0.0923	-0.0041	0.0019	0.1367	-0.0032	0.1055	6.1379	57.7438	-11.4172
6	3.0157	0.0214	-0.8723	1.0498	0.5113	2.7115	-0.0356	0.1457	-0.2026	-0.114	0.0301	-0.0655	0.21	0.0445	0.0056	0.0975	-0.0076	0.0055	0.1205	0.0029	0.1073	3.0313	51.7235	-12.3145
7	2.1607	0.8293	-0.0991	0.6111	0.406	1.188	0.0412	-0.0805	-0.1929	0.1305	-0.006	-0.0116	0.105	0.1101	-0.0352	0.0859	0.0139	0.0109	0.1319	0.0094	0.1091	-0.2033	51.8338	7.9262
8	2.2367	-0.4048	0.1288	8.5529	-0.0715	1.8798	0.0504	-0.1428	0.0371	0.2566	-0.0594	0.2407	-0.0276	-0.0992	0.009	0.0825	-0.0092	0.0172	0.162	-0.0042	0.0982	5.2413	54.9626	5.2823
9	2.1504	0.0481	0.3741	0.6358	-0.0978	0.9094	0.0488	-0.0931	0.0479	0.003	-0.0469	-0.151	0.0034	0.082	-0.0019	0.096	0.0005	0.0119	0.1439	0.0142	0.1119	-9.3838	51.3698	12.5845
10	2.3111	-1.9265	2.2383	2.5531	-0.8012	3.383	0.0272	-0.1091	-0.208	-0.0125	0.0497	0.2998	0.0253	-0.1965	-0.077	0.103	-0.0154	0.0141	0.1286	0.0203	0.1131	-31.4376	42.3987	8.3565
11	1.0475	0.7279	0.2305	2.0833	0.5931	1.3928	-0.0488	-0.2044	-0.083	0.2021	0.0633	-0.1397	0.0774	0.0052	-0.0145	0.1107	0.0321	-0.0199	0.1255	0.0277	0.0961	-19.7741	36.0895	25.9732
12	2.532	0.1293	0.0371	1.6078	0.1658	0.9235	-0.0504	-0.1541	-0.0755	0.136	0.0751	-0.0506	0.1344	0.0211	-0.0248	0.1235	0.0228	-0.0022	0.1227	0.016	0.0862	-22.0383	39.3387	23.7447
13	4.2464	0.2842	-3.5828	1.7419	0.2654	3.7455	-0.0909	-0.1995	0.1643	0.1676	0.1391	-0.0632	0.1971	0.1124	-0.0481	0.0942	0.0246	-0.0318	0.1519	0.0113	0.0763	-17.2072	46.212	28.3305
14	15.9173	-13.7174	3.3879	13.881	-1.6172	1.545	-0.0587	-0.2414	-0.845	1.2094	0.2059	0.7791	0.7188	-0.0604	-0.1472	0.6508	0.0066	0.0335	0.2363	0.0628	0.0569	-25.5827	36.6473	37.6085
15	2.2416	2.3722	-1.2265	5.6636	-1.6271	2.8216	-0.0247	-0.1896	-0.1028	0.2114	-0.0072	-0.2334	0.1258	0.1015	0.0319	0.1045	0.0298	-0.0248	0.1431	0.01	0.0853	-21.236	45.8647	28.7661
16	1.7878	0.2983	-0.2251	2.0995	-0.1333	0.5559	-0.0084	-0.0841	-0.0236	0.127	0.0186	-0.1145	-0.0318	0.0411	-0.0102	0.0973	0.0032	-0.0069	0.1423	-0.0155	0.0575	-25.5101	57.0252	24.5571
17	3.1326	1.7859	0.6269	4.3394	1.4385	1.4404	0.005	-0.2241	0.1131	0.2431	0.0453	-0.2426	-0.072	0.0502	-0.0502	0.104	0.001	-0.0212	0.1374	-0.0205	0.0863	-25.1554	59.3728	26.5837
18	2.1684	0.5116	-0.346	1.0598	0.3493	1.0645	-0.0558	0.0801	-0.0919	-0.0394	0.0306	-0.0427	0.0653	0.0089	0.0252	0.1162	0.0028	0	0.1193	0.0072	0.0897	-25.8989	54.1646	18.4777
19	10.3614	-4.4539	-2.618	3.1756	1.3223	2.2206	-0.053	0.2233	0.0117	0.0541	-0.0088	-0.0059	0.028	0.0138	0.0618	0.1094	-0.0105	-0.002	0.1288	-0.0082	0.1096	-25.8857	64.847	18.4051
20	1.1018	-0.1533	-1.6879	0.3743	0.3348	2.8553	0.032	-0.0636	0.1409	0.0076	0.0519	-0.0819	-0.0765	0.0797	-0.084	0.0916	0.0025	-0.0033	0.1359	-0.0083	0.1285	-27.3279	63.9742	19.426
21	3.2976	0.9411	-0.5749	0.9919	-0.5423	2.295	-0.0205	0.0368	0.1388	-0.047	-0.02	-0.0434	-0.0993	-0.002	0.0406	0.0968	-0.002	0.0047	0.0947	0.005	0.1039	-25.9924	62.8571	3.1741
22	3.4985	1.5735	-0.3488	3.1151	-0.7098	2.5327	0.003	0.0363	0.2065	-0.0764	-0.0544	-0.0131	-0.165	0.0297	0.0515	0.1051	0.0073	0.0016	0.127	0.0108	0.0928	-28.786	63.3219	2.4427
23	5.8472	1.6807	1.4206	2.3868	0.4354	1.4816	-0.0077	-0.0719	0.0008	-0.0266	-0.028	0.0218	0.0277	-0.041	0.0357	0.1199	0.0078	0.0122	0.1274	0.0115	0.0931	-24.3294	53.7546	4.9288
24	7.6661	-2.1709	4.3547	1.0348	-1.4401	2.7926	0.0574	0.2264	-0.3022	-0.0167	0.0274	0.092	0.001	0.1026	-0.0848	0.0822	0.0028	0.002	0.1622	0.0155	0.114	-23.7454	59.6128	-5.5892
25	3.2413	-3.4983	-0.1841	4.4691	-0.1424	0.1927	-0.0143	0.1448	0.1547	-0.0282	-0.0448	-0.2458	0.0152	-0.0184	0.0591	0.1031	-0.0045	-0.0027	0.1813	0.0291	0.1182	-25.5486	59.8551	-4.6811
26	3.456	-1.0449	-0.6193	2.6738	-0.2817	1.0598	0.049	0.2303	0.0641	-0.2866	-0.0482	-0.1987	0.1809	0.0378	-0.0008	0.0995	0.0008	0.0366	0.1393	-0.0096	0.0247	-17.8044	43.9268	-8.1779
27	1.3474	-1.8819	0.2066	2.6769	-0.1322	0.8743	0.1522	0.1301	0.1122	-0.2248	-0.1189	-0.153	0.1195	0.0799	-0.0334	0.1335	-0.0399	0.0272	0.2038	0.0159	0.0734	-23.6724	46.3301	-8.9795
28	5.047	2.1777	-3.021	2.5263	-1.8992	8.2091	-0.0175	0.4271	-0.0871	-0.3047	0.1989	-0.0706	0.231	-0.194	-0.1814	0.1258	-0.013	0.0249	0.1311	-0.0274	0.0528	-24.3697	41.2353	-9.8561
29	1.7956	0.0432	0.0814	1.3475	-0.147	0.6485	0.0051	0.1633	-0.1332	-0.1931	0.0041	-0.0857	0.1195	0.0093	-0.0092	0.1276	0.005	0.0199	0.125	-0.0058	0.0964	-19.0865	40.852	-1.9732
30	6.042	-0.682	2.8967	2.5709	-0.9117	3.9316	-0.0943	0.6335	-0.0077	-0.5059	0.0302	-0.0781	0.0267	0.2145	0.0641	0.1546	-0.0073	0.0485	0.1479	-0.0191	0.0894	-17.7374	36.3551	-6.553
31	2.354	0.6411	1.3351	3.9758	-2.247	6.3368	-0.0715	-0.0244	-0.3126	0.0755	-0.1317	-0.3083	0.2012	0.1582	0.2031	0.0719	0.0476	0.0233	0.0527	-0.0015	0.1854	-10.6458	26.9435	11.4879
32	2.3398	0.248	0.8976	1.6406	0.0746	1.8499	-0.038	0.1319	-0.1559	-0.1149	0.0293	-0.0883	0.2262	0.0582	0.0088	0.1117	0.0212	0.023	0.0911	-0.0119	0.1358	-19.3214	29.4631	2.873
33	2.1825	0.416	-0.0622	1.7085	-0.0827	0.52	0.0152	-0.0004	-0.1649	-0.0592	-0.0464	-0.0813	0.129	0.03	0.0311	0.1188	0.0155	0.0122	0.1045	0.0104	0.1085	-19.1778	32.5991	8.9471
34	4.0024	1.9098	-0.4289	6.5141	-1.2476	2.0433	0.0417	-0.0113	-0.5209	-0.113	-0.0928	-0.1611	0.2784	0.0094	0.0511	0.1178	0.0365	-0.0068	0.0732	0.022	0.1566	-15.3606	25.5607	15.6169
35	2.2103	1.0277	1.5892	1.113	0.8464	3.2182	0.072	-0.0122	-0.3205	0.0223	-0.0238	-0.2548	0.3716	0.137	-0.0482	0.1198	0.0321	0.0088	0.0851	0.023	0.1718	-15.736	27.1774	14.5801

Refinement TLS group

ID	Refine-ID	Refine TLS-ID	Auth asym-ID	Auth seq-ID
1	X-RAY DIFFRACTION	1	A	1 - 12
2	X-RAY DIFFRACTION	2	A	13 - 62
3	X-RAY DIFFRACTION	3	A	63 - 91
4	X-RAY DIFFRACTION	4	A	92 - 153
5	X-RAY DIFFRACTION	5	A	154 - 182
6	X-RAY DIFFRACTION	6	A	183 - 201
7	X-RAY DIFFRACTION	7	A	202 - 225
8	X-RAY DIFFRACTION	8	A	226 - 259
9	X-RAY DIFFRACTION	9	A	260 - 287
10	X-RAY DIFFRACTION	10	A	288 - 297
11	X-RAY DIFFRACTION	11	B	1 - 23
12	X-RAY DIFFRACTION	12	B	24 - 44
13	X-RAY DIFFRACTION	13	B	45 - 52
14	X-RAY DIFFRACTION	14	B	53 - 58
15	X-RAY DIFFRACTION	15	B	59 - 70
16	X-RAY DIFFRACTION	16	C	1 - 17
17	X-RAY DIFFRACTION	17	C	18 - 27
18	X-RAY DIFFRACTION	18	C	28 - 46
19	X-RAY DIFFRACTION	19	C	47 - 54
20	X-RAY DIFFRACTION	20	C	55 - 70
21	X-RAY DIFFRACTION	21	D	1 - 16
22	X-RAY DIFFRACTION	22	D	17 - 31
23	X-RAY DIFFRACTION	23	D	32 - 46
24	X-RAY DIFFRACTION	24	D	47 - 54
25	X-RAY DIFFRACTION	25	D	55 - 70
26	X-RAY DIFFRACTION	26	E	1 - 14
27	X-RAY DIFFRACTION	27	E	15 - 25
28	X-RAY DIFFRACTION	28	E	26 - 32
29	X-RAY DIFFRACTION	29	E	33 - 55
30	X-RAY DIFFRACTION	30	E	56 - 70
31	X-RAY DIFFRACTION	31	F	1 - 10
32	X-RAY DIFFRACTION	32	F	11 - 25
33	X-RAY DIFFRACTION	33	F	26 - 46
34	X-RAY DIFFRACTION	34	F	47 - 55
35	X-RAY DIFFRACTION	35	F	56 - 70

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