PDB-4gpk: Crystal structure of NprR in complex with its cognate peptide NprX

ID or keywords:

Entry

Database: PDB / ID: 4gpk

Title

Crystal structure of NprR in complex with its cognate peptide NprX

Components

NprR
NprX peptide

Keywords

Transcription / Peptide binding protein / TPR motif / Transcription factor / Quorum sensor / Transcription-Signaling peptide complex

Function / homology

Function and homology information

Serine Threonine Protein Phosphatase 5, Tetratricopeptide repeat - #1000 / Tetratricopeptide repeat / Tetratricopeptide repeat domain / TPR repeat profile. / Tetratricopeptide repeats / Tetratricopeptide repeat / Serine Threonine Protein Phosphatase 5, Tetratricopeptide repeat / Alpha Horseshoe / Tetratricopeptide-like helical domain superfamily / Mainly Alpha
Similarity search - Domain/homology

Biological species

Bacillus thuringiensis serovar thuringiensis (bacteria)

Method

X-RAY DIFFRACTION /

SYNCHROTRON /

SAD / Resolution: 3.2 Å

Authors

Zouhir, S. / Guimaraes, B. / Perchat, S. / Nicaise, M. / Lereclus, D. / Nessler, S.

Citation

Journal: Nucleic Acids Res. / Year: 2013
Title: Peptide-binding dependent conformational changes regulate the transcriptional activity of the quorum-sensor NprR.
Authors: Zouhir, S. / Perchat, S. / Nicaise, M. / Perez, J. / Guimaraes, B. / Lereclus, D. / Nessler, S.

History

Deposition	Aug 21, 2012	Deposition site: RCSB / Processing site: RCSB
Revision 1.0	Jul 3, 2013	Provider: repository / Type: Initial release
Revision 1.1	Sep 18, 2013	Group: Database references
Revision 1.2	Jul 17, 2019	Group: Data collection / Refinement description / Category: software Item: _software.classification / _software.contact_author ..._software.classification / _software.contact_author / _software.location / _software.name / _software.type / _software.version
Revision 1.3	Feb 28, 2024	Group: Data collection / Database references Category: chem_comp_atom / chem_comp_bond ...chem_comp_atom / chem_comp_bond / database_2 / struct_ref_seq_dif Item: _database_2.pdbx_DOI / _database_2.pdbx_database_accession / _struct_ref_seq_dif.details

Structure viewer	Molecule: MolmilJmol/JSmol

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Download

PDBx/mmCIF format	4gpk.cif.gz	840.7 KB	Display	PDBx/mmCIF format
PDB format	pdb4gpk.ent.gz	704 KB	Display	PDB format
PDBx/mmJSON format	4gpk.json.gz		Tree view	PDBx/mmJSON format
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Validation report

Summary document	4gpk_validation.pdf.gz	614.9 KB	Display	wwPDB validaton report
Full document	4gpk_full_validation.pdf.gz	674.6 KB	Display
Data in XML	4gpk_validation.xml.gz	135.7 KB	Display
Data in CIF	4gpk_validation.cif.gz	181.9 KB	Display
Arichive directory	https://data.pdbj.org/pub/pdb/validation_reports/gp/4gpk ftp://data.pdbj.org/pub/pdb/validation_reports/gp/4gpk	HTTPS FTP

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Related structure data

Similar structure data	3zur-d 10603 7bwk-d 429 3gxd-d 1ff3-4 2h6b-1 3gxm-d Search similar-shape structures by Omokage search (details) Search similar-shape structures by Omokage search (details) Search similar-shape structures by Omokage search (details) Search similar-shape structures by Omokage search (details) Similarity search - Function & homologyF&H Search Similarity search - HomologyF&H Search

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Links

PDB pages	PDBj / wwPDB / NCBI
Related items in Molecule of the Month	#141 - Sep 2011 O-GlcNAc Transferase similarity (4) #230 - Feb 2019 Initiation Factor eIF4E similarity (4) #166 - Oct 2013 Proteasome similarity (2)

Deposited unit

A: NprR

B: NprR

C: NprR

D: NprR

E: NprR

F: NprR

G: NprR

H: NprR

I: NprR

J: NprR

K: NprR

L: NprR

M: NprX peptide

N: NprX peptide

O: NprX peptide

P: NprX peptide

Q: NprX peptide

R: NprX peptide

S: NprX peptide

T: NprX peptide

U: NprX peptide

V: NprX peptide

W: NprX peptide

X: NprX peptide

544 kDa, 24 polymers
Search similar-shape structures of this assembly by Omokage search (details)

1

A: NprR

B: NprR

C: NprR

D: NprR

M: NprX peptide

N: NprX peptide

O: NprX peptide

P: NprX peptide

defined by author
181 kDa, 8 polymers
Search similar-shape structures of this assembly by Omokage search (details)

2

E: NprR

F: NprR

G: NprR

H: NprR

Q: NprX peptide

R: NprX peptide

S: NprX peptide

T: NprX peptide

defined by author
181 kDa, 8 polymers
Search similar-shape structures of this assembly by Omokage search (details)

3

I: NprR

J: NprR

K: NprR

L: NprR

U: NprX peptide

V: NprX peptide

W: NprX peptide

X: NprX peptide

defined by author
181 kDa, 8 polymers
Search similar-shape structures of this assembly by Omokage search (details)

Unit cell

Length a, b, c (Å)	122.240, 133.350, 137.500
Angle α, β, γ (deg.)	108.25, 104.83, 103.83
Int Tables number	1
Space group name H-M	P1

Details

AUTHORS STATE THAT THE BIOLOGICAL ASSEMBLY IS A TETRAMER OF NPRR, WITH A PEPTIDE BOUND IN EACH SUBUNIT.

#1: Protein	NprR Mass: 44531.219 Da / Num. of mol.: 12 Fragment: THIS IS A TRUNCATED FORM OF THE FULL-LENGTH PROTEIN, MISSING THE 60 RESIDUES OF THE N-TERMINAL HTH DOMAIN, AND WITH AN ADDITIONAL C-TERMINAL HIS-TAG Source method: isolated from a genetically manipulated source Source: (gene. exp.) Bacillus thuringiensis serovar thuringiensis (bacteria) Gene: nprR / Production host: Escherichia coli (E. coli) / References: UniProt: G5DDY8
#2: Protein/peptide	NprX peptide Mass: 802.894 Da / Num. of mol.: 12 / Source method: obtained synthetically

#1: Protein

NprR

Mass: 44531.219 Da / Num. of mol.: 12
Fragment: THIS IS A TRUNCATED FORM OF THE FULL-LENGTH PROTEIN, MISSING THE 60 RESIDUES OF THE N-TERMINAL HTH DOMAIN, AND WITH AN ADDITIONAL C-TERMINAL HIS-TAG
Source method: isolated from a genetically manipulated source
Source: (gene. exp.)

Bacillus thuringiensis serovar thuringiensis (bacteria)
Gene: nprR / Production host:

Escherichia coli (E. coli) / References: UniProt: G5DDY8

#2: Protein/peptide

NprX peptide

Mass: 802.894 Da / Num. of mol.: 12 / Source method: obtained synthetically

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Experiment

Experiment	Method: X-RAY DIFFRACTION / Number of used crystals: 2

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Sample preparation

Crystal	Density Matthews: 3.55 Å³/Da / Density % sol: 65.32 %
Crystal grow	Temperature: 291 K / Method: vapor diffusion, hanging drop / pH: 7.6 Details: 0.975M Natrium Citrate, 0.1M HEPES, pH 7.6, VAPOR DIFFUSION, HANGING DROP, temperature 291K

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Data collection

Diffraction

ID	Mean temperature (K)	Crystal-ID
1	100	1
2	100	1

Diffraction source

Source	Site	Beamline	ID	Wavelength (Å)
SYNCHROTRON	SOLEIL	PROXIMA 1	1	0.97918
SYNCHROTRON	SOLEIL	PROXIMA 1	2	0.98011

Detector

Type	ID	Detector	Date	Details
ADSC QUANTUM 315r	1	CCD	Feb 3, 2010
DECTRIS PILATUS 6M	2	PIXEL	Nov 27, 2011	Kirkpatrick-Baez pair of bi-morph mirrors plus channel cut cryogenically cooled monochromator crystal

Radiation

ID	Monochromator	Protocol	Monochromatic (M) / Laue (L)	Scattering type	Wavelength-ID
1	channel cut Si111	SINGLE WAVELENGTH	M	x-ray	1
2	channel cut Si111	SINGLE WAVELENGTH	M	x-ray	2

Radiation wavelength

ID	Wavelength (Å)	Relative weight
1	0.97918	1
2	0.98011	1

Reflection

Number: 715889 / R_merge(I) obs: 0.098 / D res high: 3.47 Å / Num. obs: 187712 / % possible obs: 96.2

Diffraction reflection shell

Highest resolution (Å)	Lowest resolution (Å)	Num. obs	% possible obs (%)	ID	R_merge(I) obs
3.47	3.68	27788	88.4	1	0.706
3.68	3.93	28840	97.8	1	0.442
3.93	4.24	26890	97.8	1	0.243
4.24	4.64	24732	97.9	1	0.127
4.64	5.18	22380	97.8	1	0.105
5.18	5.97	19826	97.9	1	0.112
5.97	7.28	16775	97.5	1	0.07
7.28	10.16	13014	97.4	1	0.041

Reflection

Resolution: 3.09→50 Å / Num. all: 132686 / Num. obs: 132663 / % possible obs: 97 % / Observed criterion σ(F): -3 / Observed criterion σ(I): -3 / Redundancy: 3.9 % / B_iso Wilson estimate: 110.33 Å² / R_merge(I) obs: 0.045 / Net I/σ(I): 16.87

Reflection shell

Resolution (Å)	R_merge(I) obs	Mean I/σ(I) obs	Diffraction-ID	% possible all
3.09-3.28	0.643	1.95	1,2	94.5
3.28-3.51	0.274	4.57	1,2	97.5
3.51-3.79	0.135	8.85	1,2	97.6
3.79-4.14	0.075	15.34	1,2	97.8
4.14-4.63	0.046	24.29	1,2	97.8
4.63-5.34	0.041	28.27	1,2	97.6
5.34-6.52	0.04	30.02	1,2	97.6
6.52-9.14	0.031	37.56	1,2	97.1
9.14-50	0.029	40.6	1,2	95.4

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Phasing

Phasing

Method:

SAD

Phasing MAD set site

ID	Cartn x (Å)	Cartn y (Å)	Cartn z (Å)	Atom type symbol	B iso	Occupancy
1	68.815	54.226	99.678	S	20	1
2	65.574	60.29	120.077	S	20	0.82
3	87.094	26.15	173.068	S	20	0.814
4	64.814	22.494	108.774	S	20	0.806
5	63.907	65.689	130.322	S	20	0.795
6	24.219	55.673	145.395	S	20	0.793
7	57.33	30.684	111.052	S	20	0.782
8	117.333	1.86	176.295	S	20	0.775
9	89.948	23.749	123.728	S	20	0.77
10	73.299	51.684	89.813	S	20	0.736
11	38.271	78.591	169.753	S	20	0.721
12	32.23	72.483	176.102	S	20	0.719
13	59.697	60.018	102.722	S	20	0.716
14	77.859	27.372	166.611	S	20	0.708
15	28.681	61.933	174.412	S	20	0.708
16	33.171	51.039	116.335	S	20	0.705
17	94.524	-1.66	156.574	S	20	0.704
18	14.466	64.688	157.07	S	20	0.702
19	19.614	77.412	140.672	S	20	0.693
20	39.095	43.652	87.986	S	20	0.684
21	112.964	10.031	169.543	S	20	0.679
22	42.356	45.306	113.039	S	20	0.667
23	33.338	115.963	181.315	S	20	0.663
24	59.814	30.988	137.411	S	20	0.657
25	23.857	87.091	157.249	S	20	0.655
26	38.953	90.88	183.01	S	20	0.651
27	1.847	85.603	174.362	S	20	0.637
28	109.488	26.455	156.918	S	20	0.622
29	29.582	74.745	99.531	S	20	0.621
30	103.475	29.588	186.452	S	20	0.616
31	-1.701	84.896	202.923	S	20	0.591
32	97.899	-14.327	187.714	S	20	0.582
33	73.132	3.078	150.612	S	20	0.581
34	103.41	10.815	163.303	S	20	0.575
35	21.474	89.249	202.543	S	20	0.573
36	29.629	86.822	187.54	S	20	0.569
37	50.495	71.38	93.072	S	20	0.569
38	22.141	83.963	205.518	S	20	0.566
39	50.394	73.737	158.384	S	20	0.554
40	27.147	97.906	158.461	S	20	0.553
41	71.309	51.03	117.478	S	20	0.548
42	46.945	43.648	103.131	S	20	0.547
43	51.47	76.948	94.753	S	20	0.546
44	34.864	104.711	153.58	S	20	0.542
45	133.299	36.311	167.821	S	20	0.542
46	24.788	78.186	143.428	S	20	0.54
47	10.982	89.778	170.054	S	20	0.535
48	52.695	94.76	158.538	S	20	0.534
49	85.806	54.43	83.995	S	20	0.534
50	128.751	39.132	168.291	S	20	0.525
51	91.501	17.543	178.162	S	20	0.514
52	20.865	82.476	88.232	S	20	0.509
53	71.996	88.391	115.752	S	20	0.508
54	84.601	16.26	148.281	S	20	0.504
55	17.189	98.028	174.654	S	20	0.5
56	116.3	29.093	166.108	S	20	0.499
57	83.393	3.498	184.355	S	20	0.488
58	50.654	51.114	140.475	S	20	0.488
59	84.142	31.65	109.604	S	20	0.487
60	95.069	-2.61	150.244	S	20	0.487
61	106.423	53.657	178.964	S	20	0.467
62	56.93	36.8	120.858	S	20	0.463
63	40.102	71.621	112.627	S	20	0.461
64	107.799	62.071	158.82	S	20	0.458
65	105.023	1.592	192.433	S	20	0.454
66	102.939	35.584	178.403	S	20	0.449
67	45.822	99.231	187.504	S	20	0.447
68	54.862	29.874	140.117	S	20	0.446
69	-12.644	82.524	166.459	S	20	0.442
70	32.439	118.112	147.063	S	20	0.441
71	82.933	2.691	189.46	S	20	0.441
72	65.107	80.145	132.398	S	20	0.441
73	39.829	57.456	199.516	S	20	0.437
74	85.54	45.201	126.324	S	20	0.435
75	96.622	64.896	99.164	S	20	0.434
76	28.883	50.606	183.981	S	20	0.433
77	90.285	45.934	124.137	S	20	0.428
78	59.897	36.357	83.162	S	20	0.426
79	61.575	9.842	102.805	S	20	0.418
80	21.309	47.962	125.29	S	20	0.417
81	100.05	109.842	132.047	S	20	0.415
82	83.197	74.777	107.637	S	20	0.414
83	67.694	37.944	167.905	S	20	0.41
84	24.533	27.735	129.137	S	20	0.41
85	1.306	81.394	88.575	S	20	0.407
86	53.458	46.557	70.173	S	20	0.395
87	37.599	37.425	85.585	S	20	0.395
88	55.573	74.057	160.06	S	20	0.394
89	11.915	110.015	184.583	S	20	0.392
90	34.435	23.225	117.564	S	20	0.389
91	116.561	13.249	131.344	S	20	0.386
92	128.062	27.357	187.441	S	20	0.385
93	109.45	31.765	133.903	S	20	0.384
94	15.355	99.973	188.985	S	20	0.379
95	133.981	44.492	189.719	S	20	0.366
96	109.062	29.534	196.114	S	20	0.355
97	49.832	72.621	171.381	S	20	0.351
98	111.687	59.546	155.242	S	20	0.35
99	100.626	56.693	179.253	S	20	0.348
100	-5.495	89.121	73.623	S	20	0.343
101	3.786	106.082	153.279	S	20	0.33
102	88.54	6.343	198.233	S	20	0.324
103	-1.116	78.059	81.027	S	20	0.316
104	11.483	115.585	182.534	S	20	0.311
105	41.729	9.39	101.14	S	20	0.309
106	62.551	47.181	152.144	S	20	0.306
107	138.46	1.8	156.681	S	20	0.302
108	-8.983	92.257	148.526	S	20	0.297
109	31.49	35.655	82.097	S	20	0.294
110	14.481	122.182	150.104	S	20	0.293
111	27.941	101.535	118.993	S	20	0.289
112	58.449	106.499	159.808	S	20	0.289
113	47.099	69.756	194.322	S	20	0.289
114	96.021	19.673	190.58	S	20	0.282
115	137.332	49.193	202.196	S	20	0.282
116	48.247	94.266	137.062	S	20	0.282
117	95.145	44.814	74.762	S	20	0.282
118	-20.18	76.003	179.689	S	20	0.279
119	132.403	-3.685	174.839	S	20	0.277
120	53.262	24.461	130.497	S	20	0.276
121	48.776	-0.949	114.504	S	20	0.271
122	30.701	-21.969	107.708	S	20	0.27
123	93.739	11.061	187.963	S	20	0.267
124	16.688	60.228	169.763	S	20	0.266
125	49.296	40.219	98.07	S	20	0.265
126	106.371	8.45	193.434	S	20	0.261
127	54.095	78.021	204.01	S	20	0.261
128	104.238	22.528	156.864	S	20	0.26
129	11.332	101.489	199.259	S	20	0.258
130	94.652	48.653	158.354	S	20	0.257
131	7.752	75.724	192.369	S	20	0.256
132	108.844	11.974	111.26	S	20	0.249
133	25.193	93.121	163.447	S	20	0.247
134	56.378	76.953	148.753	S	20	0.247
135	107.936	34.5	148.561	S	20	0.245
136	97.948	62.385	91.942	S	20	0.244
137	86.549	71.616	120.917	S	20	0.243
138	82.172	-7.465	172.728	S	20	0.239
139	92.272	64.617	177.774	S	20	0.238
140	33.993	75.964	204.19	S	20	0.237
141	46.035	76.289	168.303	S	20	0.23
142	92.536	-29.48	189.759	S	20	0.227
143	104.752	125.368	136.933	S	20	0.226
144	118.239	49.855	155.28	S	20	0.219
145	51.182	54.555	64.224	S	20	0.218
146	149.527	38.543	212.724	S	20	0.218
147	114.368	25.107	187.804	S	20	0.217
148	25.151	73.364	128.639	S	20	0.206
149	50.73	24.874	137.466	S	20	0.206
150	95.571	17.046	116.106	S	20	0.205
151	27.501	102.789	169.889	S	20	0.205
152	-4.794	87.403	191.246	S	20	0.204
153	51.924	72.238	194.32	S	20	0.203
154	122.494	-4.997	154.779	S	20	0.197
155	19.248	99.039	209.285	S	20	0.193
156	27.47	87.683	172.701	S	20	0.192
157	29.79	105.29	150.006	S	20	0.189
158	145.062	-5.967	153.063	S	20	0.188
159	113.957	40.72	162.012	S	20	0.187
160	22.589	74.689	167.002	S	20	0.187
161	38.663	-14.672	83.22	S	20	0.186
162	132.092	3.649	165.824	S	20	0.185
163	48.609	63.056	125.929	S	20	0.184
164	13.016	66.019	107.555	S	20	0.184
165	69.615	43.233	126.125	S	20	0.182
166	44.492	24.62	180.009	S	20	0.181
167	-29.939	99.624	168.129	S	20	0.18
168	16.683	65.053	148.518	S	20	0.178
169	72.527	-1.242	183.129	S	20	0.177
170	19.581	55.985	151.14	S	20	0.175
171	-11.625	101.107	172.352	S	20	0.174
172	46.181	13.408	103.94	S	20	0.173
173	136.805	38.869	210.723	S	20	0.172
174	133.832	25.29	181.243	S	20	0.158
175	77.42	12.122	186.007	S	20	0.157
176	12.546	40.239	149.914	S	20	0.154
177	85.68	3.766	174.682	S	20	0.152
178	-4.957	84.968	86.313	S	20	0.15
179	17.218	66.817	118.809	S	20	0.149
180	43.573	47.059	84.802	S	20	0.147
181	153.43	-7.412	146.955	S	20	0.145
182	60.135	42.339	62.395	S	20	0.142
183	84.064	67.276	163.657	S	20	0.14
184	46.212	5.729	184.717	S	20	0.14
185	38.377	-25.841	96.712	S	20	0.137
186	92.925	-14.406	192.96	S	20	0.131
187	106.006	19.299	99.619	S	20	0.13
188	107.149	58.509	109.691	S	20	0.13
189	2.737	73.807	92.803	S	20	0.129
190	24.474	31.005	122.18	S	20	0.122
191	128.291	39.064	176.531	S	20	0.104
192	40.851	14.951	197.656	S	20	0.091
193	58.82	51.241	215.819	S	20	0.091
194	-8.371	82.209	129.272	S	20	0.081
195	-15.211	100.663	179.601	S	20	0.064
196	33.756	46.64	71.836	S	20	0.02

Phasing dm

FOM : 0.78 / FOM acentric: 0.78 / FOM centric: 0 / Reflection: 94307 / Reflection acentric: 94307 / Reflection centric: 0

Phasing dm shell

Resolution (Å)	FOM	FOM acentric	Reflection	Reflection acentric
9.9-44.448	0.94	0.94	4042	4042
6.2-9.9	0.91	0.91	12768	12768
5-6.2	0.82	0.82	16002	16002
4.3-5	0.81	0.81	16234	16234
3.7-4.3	0.72	0.72	28748	28748
3.5-3.7	0.66	0.66	16513	16513

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Processing

Software

Name	Version	Classification
PHENIX	1.8_1069	refinement
SHELX		phasing
RESOLVE	2.13	phasing
BUSTER-TNT		refinement
PDB_EXTRACT	3.11	data extraction
ADSC	Quantum	data collection
SHELXD		phasing
XSCALE		data scaling

Refinement

Method to determine structure:

SAD / Resolution: 3.2→29.736 Å / Cor.coef. F_o:F_c: 0.952 / Cor.coef. F_o:F_c free: 0.9327 / Occupancy max: 1 / Occupancy min: 1 / SU ML: 0.51 / σ(F): 1.99 / Phase error: 34.67 / Stereochemistry target values: ML

	R_factor	Num. reflection	% reflection
R_free	0.2994	24324	20 %
R_work	0.2695	-	-
obs	0.2755	121622	98.46 %
all	-	132655	-

Solvent computation

Shrinkage radii: 0.9 Å / VDW probe radii: 1.11 Å / Solvent model: FLAT BULK SOLVENT MODEL

Displacement parameters

B_iso mean: 159.96 Å²

	B_aniso -1	B_aniso -2	B_aniso -3
1-	-15.7013 Å²	-0.4954 Å²	-4.416 Å²
2-	-	2.7796 Å²	5.4622 Å²
3-	-	-	12.9218 Å²

Refine analyze

Luzzati coordinate error obs: 1.42 Å

Refinement step

Cycle: LAST / Resolution: 3.2→29.736 Å

	Protein	Nucleic acid	Ligand	Solvent	Total
Num. atoms	35360	0	0	0	35360

Refine LS restraints

Refine-ID	Type	Dev ideal	Number
X-RAY DIFFRACTION	f_bond_d	0.002	36040
X-RAY DIFFRACTION	f_angle_d	0.632	48431
X-RAY DIFFRACTION	f_dihedral_angle_d	12.483	13753
X-RAY DIFFRACTION	f_chiral_restr	0.05	5230
X-RAY DIFFRACTION	f_plane_restr	0.002	6029

LS refinement shell

Resolution (Å)	R_factor R_free	Num. reflection R_free	R_factor R_work	Num. reflection R_work	Refine-ID	% reflection obs (%)
3.2-3.2331	0.3976	747	0.3493	2990	X-RAY DIFFRACTION	91
3.2331-3.2711	0.4004	812	0.3493	3248	X-RAY DIFFRACTION	99
3.2711-3.311	0.3795	811	0.322	3243	X-RAY DIFFRACTION	98
3.311-3.3528	0.3675	817	0.3209	3269	X-RAY DIFFRACTION	99
3.3528-3.3969	0.3504	808	0.316	3230	X-RAY DIFFRACTION	99
3.3969-3.4433	0.3737	815	0.3151	3262	X-RAY DIFFRACTION	99
3.4433-3.4925	0.3585	815	0.325	3259	X-RAY DIFFRACTION	99
3.4925-3.5445	0.3642	809	0.3156	3235	X-RAY DIFFRACTION	99
3.5445-3.5998	0.3541	828	0.3079	3311	X-RAY DIFFRACTION	99
3.5998-3.6587	0.3278	796	0.3124	3187	X-RAY DIFFRACTION	99
3.6587-3.7217	0.3402	817	0.2944	3265	X-RAY DIFFRACTION	99
3.7217-3.7892	0.3575	817	0.3078	3267	X-RAY DIFFRACTION	99
3.7892-3.862	0.353	813	0.3065	3253	X-RAY DIFFRACTION	99
3.862-3.9406	0.3473	822	0.3054	3285	X-RAY DIFFRACTION	99
3.9406-4.0261	0.3325	806	0.2977	3227	X-RAY DIFFRACTION	99
4.0261-4.1195	0.3466	807	0.2977	3230	X-RAY DIFFRACTION	99
4.1195-4.2223	0.2979	819	0.2838	3277	X-RAY DIFFRACTION	99
4.2223-4.3361	0.3128	808	0.2895	3233	X-RAY DIFFRACTION	99
4.3361-4.4633	0.3116	823	0.2821	3288	X-RAY DIFFRACTION	99
4.4633-4.6068	0.2977	816	0.2698	3264	X-RAY DIFFRACTION	99
4.6068-4.7708	0.2943	821	0.2693	3286	X-RAY DIFFRACTION	99
4.7708-4.961	0.3212	816	0.2712	3263	X-RAY DIFFRACTION	99
4.961-5.1857	0.3183	807	0.2896	3231	X-RAY DIFFRACTION	99
5.1857-5.4575	0.3409	817	0.2945	3265	X-RAY DIFFRACTION	99
5.4575-5.7971	0.3379	811	0.3218	3243	X-RAY DIFFRACTION	99
5.7971-6.2409	0.3575	813	0.3169	3252	X-RAY DIFFRACTION	99
6.2409-6.8619	0.3147	813	0.2805	3256	X-RAY DIFFRACTION	98
6.8619-7.8389	0.2487	809	0.2292	3236	X-RAY DIFFRACTION	99
7.8389-9.8168	0.2047	810	0.1936	3237	X-RAY DIFFRACTION	98
9.8168-29.7373	0.2375	801	0.2179	3206	X-RAY DIFFRACTION	97

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