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- PDB-3zxs: Cryptochrome B from Rhodobacter sphaeroides -

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Basic information

Entry
Database: PDB / ID: 3zxs
TitleCryptochrome B from Rhodobacter sphaeroides
ComponentsCRYPTOCHROME B
KeywordsLYASE / CRYPRO / LUMAZINE / IRON-SULFUR-CLUSTER
Function / homology
Function and homology information


4 iron, 4 sulfur cluster binding / lyase activity / nucleotide binding / metal ion binding
Similarity search - Function
Deoxyribodipyrimidine photolyase-related / Photolyase PhrB-like / Deoxyribodipyrimidine photo-lyase-related protein / DNA Cyclobutane Dipyrimidine Photolyase, subunit A; domain 3 / DNA Cyclobutane Dipyrimidine Photolyase, subunit A, domain 3 / Serine Threonine Protein Phosphatase 5, Tetratricopeptide repeat - #80 / Cryptochrome/DNA photolyase, FAD-binding domain-like superfamily / HUPs / Rossmann-like alpha/beta/alpha sandwich fold / Serine Threonine Protein Phosphatase 5, Tetratricopeptide repeat ...Deoxyribodipyrimidine photolyase-related / Photolyase PhrB-like / Deoxyribodipyrimidine photo-lyase-related protein / DNA Cyclobutane Dipyrimidine Photolyase, subunit A; domain 3 / DNA Cyclobutane Dipyrimidine Photolyase, subunit A, domain 3 / Serine Threonine Protein Phosphatase 5, Tetratricopeptide repeat - #80 / Cryptochrome/DNA photolyase, FAD-binding domain-like superfamily / HUPs / Rossmann-like alpha/beta/alpha sandwich fold / Serine Threonine Protein Phosphatase 5, Tetratricopeptide repeat / Alpha Horseshoe / Arc Repressor Mutant, subunit A / Rossmann fold / Orthogonal Bundle / 3-Layer(aba) Sandwich / Mainly Alpha / Alpha Beta
Similarity search - Domain/homology
Chem-DLZ / FLAVIN-ADENINE DINUCLEOTIDE / GADOLINIUM ATOM / IRON/SULFUR CLUSTER / Deoxyribodipyrimidine photolyase-related protein
Similarity search - Component
Biological speciesRHODOBACTER SPHAEROIDES (bacteria)
MethodX-RAY DIFFRACTION / SYNCHROTRON / SAD / Resolution: 2.7 Å
AuthorsGeisselbrecht, Y. / Fruhwirth, S. / Pierik, A.J. / Klug, G. / Essen, L.-O.
CitationJournal: Embo Rep. / Year: 2012
Title: Cryb from Rhodobacter Sphaeroides: A Unique Class of Cryptochromes with New Cofactors.
Authors: Geisselbrecht, Y. / Fruhwirth, S. / Schroeder, C. / Pierik, A.J. / Klug, G. / Essen, L.-O.
History
DepositionAug 15, 2011Deposition site: PDBE / Processing site: PDBE
Revision 1.0Feb 15, 2012Provider: repository / Type: Initial release
Revision 1.1Mar 28, 2012Group: Other
Revision 1.2Aug 13, 2014Group: Refinement description
Revision 1.3May 8, 2024Group: Data collection / Database references ...Data collection / Database references / Derived calculations / Other / Refinement description
Category: chem_comp_atom / chem_comp_bond ...chem_comp_atom / chem_comp_bond / database_2 / pdbx_database_status / pdbx_struct_conn_angle / struct_conn / struct_ncs_dom_lim / struct_site
Item: _database_2.pdbx_DOI / _database_2.pdbx_database_accession ..._database_2.pdbx_DOI / _database_2.pdbx_database_accession / _pdbx_database_status.status_code_sf / _pdbx_struct_conn_angle.ptnr1_auth_comp_id / _pdbx_struct_conn_angle.ptnr1_auth_seq_id / _pdbx_struct_conn_angle.ptnr1_label_asym_id / _pdbx_struct_conn_angle.ptnr1_label_atom_id / _pdbx_struct_conn_angle.ptnr1_label_comp_id / _pdbx_struct_conn_angle.ptnr1_label_seq_id / _pdbx_struct_conn_angle.ptnr2_auth_comp_id / _pdbx_struct_conn_angle.ptnr2_auth_seq_id / _pdbx_struct_conn_angle.ptnr2_label_asym_id / _pdbx_struct_conn_angle.ptnr2_label_atom_id / _pdbx_struct_conn_angle.ptnr2_label_comp_id / _pdbx_struct_conn_angle.ptnr3_auth_comp_id / _pdbx_struct_conn_angle.ptnr3_auth_seq_id / _pdbx_struct_conn_angle.ptnr3_label_asym_id / _pdbx_struct_conn_angle.ptnr3_label_atom_id / _pdbx_struct_conn_angle.ptnr3_label_comp_id / _pdbx_struct_conn_angle.ptnr3_label_seq_id / _pdbx_struct_conn_angle.value / _struct_conn.pdbx_dist_value / _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.ptnr1_label_seq_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 / _struct_conn.ptnr2_label_seq_id / _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 / _struct_site.pdbx_auth_asym_id / _struct_site.pdbx_auth_comp_id / _struct_site.pdbx_auth_seq_id

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Structure visualization

Structure viewerMolecule:
MolmilJmol/JSmol

Downloads & links

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Assembly

Deposited unit
A: CRYPTOCHROME B
B: CRYPTOCHROME B
C: CRYPTOCHROME B
hetero molecules


Theoretical massNumber of molelcules
Total (without water)184,42018
Polymers179,4853
Non-polymers4,93515
Water7,512417
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A: CRYPTOCHROME B
hetero molecules


Theoretical massNumber of molelcules
Total (without water)61,4736
Polymers59,8281
Non-polymers1,6455
Water181
TypeNameSymmetry operationNumber
identity operation1_555x,y,z1
MethodPISA
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B: CRYPTOCHROME B
hetero molecules


Theoretical massNumber of molelcules
Total (without water)61,4736
Polymers59,8281
Non-polymers1,6455
Water181
TypeNameSymmetry operationNumber
identity operation1_555x,y,z1
MethodPISA
3
C: CRYPTOCHROME B
hetero molecules


Theoretical massNumber of molelcules
Total (without water)61,4736
Polymers59,8281
Non-polymers1,6455
Water181
TypeNameSymmetry operationNumber
identity operation1_555x,y,z1
MethodPISA
Unit cell
Length a, b, c (Å)137.840, 137.840, 521.940
Angle α, β, γ (deg.)90.00, 90.00, 120.00
Int Tables number179
Space group name H-MP6522
Noncrystallographic symmetry (NCS)NCS domain:
IDEns-IDDetails
11A
21B
31C

NCS domain segments:

Ens-ID: 1

Dom-IDComponent-IDBeg auth comp-IDBeg label comp-IDEnd auth comp-IDEnd label comp-IDRefine codeAuth asym-IDLabel asym-IDAuth seq-IDLabel seq-ID
11ARGARGGLYGLY3AA3 - 9517 - 109
21ARGARGGLYGLY3BB3 - 9517 - 109
31ARGARGGLYGLY3CC3 - 9517 - 109
12ARGARGGLUGLU3AA97 - 140111 - 154
22ARGARGGLUGLU3BB97 - 140111 - 154
32ARGARGGLUGLU3CC97 - 140111 - 154
13ARGARGPROPRO4AA146 - 184160 - 198
23ARGARGPROPRO4BB146 - 184160 - 198
33ARGARGPROPRO4CC146 - 184160 - 198
14PROPROGLNGLN4AA189 - 475203 - 489
24PROPROGLNGLN4BB189 - 475203 - 489
34PROPROGLNGLN4CC189 - 475203 - 489
15TYRTYRVALVAL4AA477 - 508491 - 522
25TYRTYRVALVAL4BB477 - 508491 - 522
35TYRTYRVALVAL4CC477 - 508491 - 522

NCS oper:
IDCodeMatrixVector
1given(-0.4936, 0.8694, 0.02437), (0.7614, 0.4455, -0.4709), (-0.4203, -0.2139, -0.8818)1.233, 170.6, 595.3
2given(-0.4936, 0.8694, 0.02437), (0.7614, 0.4455, -0.4709), (-0.4203, -0.2139, -0.8818)1.233, 170.6, 595.3
3given(-0.4936, 0.8694, 0.02437), (0.7614, 0.4455, -0.4709), (-0.4203, -0.2139, -0.8818)1.233, 170.6, 595.3
4given(-0.4936, 0.8694, 0.02437), (0.7614, 0.4455, -0.4709), (-0.4203, -0.2139, -0.8818)1.233, 170.6, 595.3
5given(-0.4936, 0.8694, 0.02437), (0.7614, 0.4455, -0.4709), (-0.4203, -0.2139, -0.8818)1.233, 170.6, 595.3
6given(-0.1318, -0.2137, 0.968), (-0.248, -0.9383, -0.2409), (0.9597, -0.2718, 0.07066)-255.4, 138.8, 263.1
7given(-0.1318, -0.2137, 0.968), (-0.248, -0.9383, -0.2409), (0.9597, -0.2718, 0.07066)-255.4, 138.8, 263.1
8given(-0.1318, -0.2137, 0.968), (-0.248, -0.9383, -0.2409), (0.9597, -0.2718, 0.07066)-255.4, 138.8, 263.1
9given(-0.1318, -0.2137, 0.968), (-0.248, -0.9383, -0.2409), (0.9597, -0.2718, 0.07066)-255.4, 138.8, 263.1
10given(-0.1318, -0.2137, 0.968), (-0.248, -0.9383, -0.2409), (0.9597, -0.2718, 0.07066)-255.4, 138.8, 263.1

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Components

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Protein , 1 types, 3 molecules ABC

#1: Protein CRYPTOCHROME B / RSCRYB


Mass: 59828.379 Da / Num. of mol.: 3 / Fragment: RESIDUES 2-508
Source method: isolated from a genetically manipulated source
Source: (gene. exp.) RHODOBACTER SPHAEROIDES (bacteria) / Strain: DSM 158 / Production host: ESCHERICHIA COLI (E. coli) / Strain (production host): JM109 / References: UniProt: Q3IXP1

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Non-polymers , 6 types, 432 molecules

#2: Chemical ChemComp-FAD / FLAVIN-ADENINE DINUCLEOTIDE / Flavin adenine dinucleotide


Mass: 785.550 Da / Num. of mol.: 3 / Source method: obtained synthetically / Formula: C27H33N9O15P2 / Comment: FAD*YM
#3: Chemical ChemComp-SF4 / IRON/SULFUR CLUSTER / Iron–sulfur cluster


Mass: 351.640 Da / Num. of mol.: 3 / Source method: obtained synthetically / Formula: Fe4S4
#4: Chemical ChemComp-DLZ / 1-deoxy-1-(6,7-dimethyl-2,4-dioxo-3,4-dihydropteridin-8(2H)-yl)-D-ribitol / 6,7-dimethyl-8-(1'-D-ribityl) lumazine / 6,7-Dimethyl-8-ribityllumazine


Mass: 326.305 Da / Num. of mol.: 3 / Source method: obtained synthetically / Formula: C13H18N4O6
#5: Chemical ChemComp-MG / MAGNESIUM ION


Mass: 24.305 Da / Num. of mol.: 3 / Source method: obtained synthetically / Formula: Mg
#6: Chemical ChemComp-GD / GADOLINIUM ATOM


Mass: 157.250 Da / Num. of mol.: 3 / Source method: obtained synthetically / Formula: Gd
#7: Water ChemComp-HOH / water / Water


Mass: 18.015 Da / Num. of mol.: 417 / Source method: isolated from a natural source / Formula: H2O

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Details

Sequence detailsHIS-TAG SEQUENCE MRGSHHHHHHGIR (RESIDUES -12-0 INSERTION OF A LEUCINE AT POSITION 2 DUE TO CLONING STRATEGY.

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Experimental details

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Experiment

ExperimentMethod: X-RAY DIFFRACTION / Number of used crystals: 1

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Sample preparation

CrystalDensity Matthews: 4.17 Å3/Da / Density % sol: 70.49 %
Description: FINE SLICING 0.06 DEGREES ROTATION DUE TO LONG C- AXIS. ANOMALOUS SIGNAL OF 4FE4S-CLUSTER USED.
Crystal growpH: 8.5
Details: 0.3 M MGCL2, 0.1M BICINE PH 8.5, 29.5% PEG2000, 17.5% GLYCEROL

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Data collection

DiffractionMean temperature: 100 K
Diffraction sourceSource: SYNCHROTRON / Site: ESRF / Beamline: ID14-4 / Wavelength: 1.319
DetectorType: ADSC QUANTUM 315r / Detector: CCD / Date: Nov 18, 2009 / Details: TORODIAL FOCUSING MIRROR
RadiationMonochromator: CHANNEL CUT ESRF MONOCHROMATOR / Protocol: SINGLE WAVELENGTH / Monochromatic (M) / Laue (L): M / Scattering type: x-ray
Radiation wavelengthWavelength: 1.319 Å / Relative weight: 1
ReflectionResolution: 2.7→25 Å / Num. obs: 81535 / % possible obs: 99.8 % / Observed criterion σ(I): -3 / Redundancy: 15.2 % / Biso Wilson estimate: 48.5 Å2 / Rmerge(I) obs: 0.1 / Net I/σ(I): 26.9
Reflection shellResolution: 2.7→2.77 Å / Redundancy: 15.2 % / Rmerge(I) obs: 0.56 / Mean I/σ(I) obs: 5.4 / % possible all: 99.8

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Processing

Software
NameVersionClassification
REFMAC5.5.0109refinement
XDSdata reduction
XSCALEdata scaling
PHENIXphasing
RefinementMethod to determine structure: SAD
Starting model: NONE

Resolution: 2.7→24.95 Å / Cor.coef. Fo:Fc: 0.931 / Cor.coef. Fo:Fc free: 0.913 / SU B: 16.371 / SU ML: 0.174 / Cross valid method: THROUGHOUT / ESU R: 0.356 / ESU R Free: 0.248
Stereochemistry target values: MAXIMUM LIKELIHOOD WITH PHASES
Details: HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS. U VALUES WITH TLS ADDED. IN MOLECULE C LOOP AA 142-144 IS DISORDERED DUE TO LACK OF ELECTRON DENSITY AND LOOP AA 183-187 SHOWS WEAK ELECTRON DENSITY.
RfactorNum. reflection% reflectionSelection details
Rfree0.22837 2000 2.5 %SHELLED
Rwork0.19774 ---
obs0.19851 79535 100 %-
Solvent computationIon probe radii: 0.8 Å / Shrinkage radii: 0.8 Å / VDW probe radii: 1.4 Å / Solvent model: MASK
Displacement parametersBiso mean: 32.223 Å2
Baniso -1Baniso -2Baniso -3
1-1.63 Å20.82 Å20 Å2
2--1.63 Å20 Å2
3----2.45 Å2
Refinement stepCycle: LAST / Resolution: 2.7→24.95 Å
ProteinNucleic acidLigandSolventTotal
Num. atoms11977 0 258 417 12652
Refine LS restraints
Refine-IDTypeDev idealDev ideal targetNumber
X-RAY DIFFRACTIONr_bond_refined_d0.0160.02112585
X-RAY DIFFRACTIONr_bond_other_d0.0010.028642
X-RAY DIFFRACTIONr_angle_refined_deg1.5461.98317174
X-RAY DIFFRACTIONr_angle_other_deg1.101320690
X-RAY DIFFRACTIONr_dihedral_angle_1_deg6.1551517
X-RAY DIFFRACTIONr_dihedral_angle_2_deg28.94821.692597
X-RAY DIFFRACTIONr_dihedral_angle_3_deg17.039151893
X-RAY DIFFRACTIONr_dihedral_angle_4_deg21.18115153
X-RAY DIFFRACTIONr_chiral_restr0.0880.21806
X-RAY DIFFRACTIONr_gen_planes_refined0.0070.02114079
X-RAY DIFFRACTIONr_gen_planes_other0.0010.022815
X-RAY DIFFRACTIONr_nbd_refined
X-RAY DIFFRACTIONr_nbd_other
X-RAY DIFFRACTIONr_nbtor_refined
X-RAY DIFFRACTIONr_nbtor_other
X-RAY DIFFRACTIONr_xyhbond_nbd_refined
X-RAY DIFFRACTIONr_xyhbond_nbd_other
X-RAY DIFFRACTIONr_metal_ion_refined
X-RAY DIFFRACTIONr_metal_ion_other
X-RAY DIFFRACTIONr_symmetry_vdw_refined
X-RAY DIFFRACTIONr_symmetry_vdw_other
X-RAY DIFFRACTIONr_symmetry_hbond_refined
X-RAY DIFFRACTIONr_symmetry_hbond_other
X-RAY DIFFRACTIONr_symmetry_metal_ion_refined
X-RAY DIFFRACTIONr_symmetry_metal_ion_other
X-RAY DIFFRACTIONr_mcbond_it0.7931.57601
X-RAY DIFFRACTIONr_mcbond_other0.2061.53039
X-RAY DIFFRACTIONr_mcangle_it1.586212099
X-RAY DIFFRACTIONr_mcangle_other
X-RAY DIFFRACTIONr_scbond_it2.38334984
X-RAY DIFFRACTIONr_scbond_other
X-RAY DIFFRACTIONr_scangle_it4.0764.55039
X-RAY DIFFRACTIONr_scangle_other
X-RAY DIFFRACTIONr_long_range_B_refined
X-RAY DIFFRACTIONr_long_range_B_other
X-RAY DIFFRACTIONr_rigid_bond_restr
X-RAY DIFFRACTIONr_sphericity_free
X-RAY DIFFRACTIONr_sphericity_bonded
Refine LS restraints NCS

Ens-ID: 1 / Refine-ID: X-RAY DIFFRACTION

Dom-IDAuth asym-IDNumberTypeRms dev position (Å)Weight position
1A804tight positional0.130.05
2B804tight positional0.110.05
3C804tight positional0.160.05
1A4745medium positional0.470.5
2B4745medium positional0.430.5
3C4745medium positional0.490.5
1A974loose positional0.415
2B974loose positional0.485
3C974loose positional0.515
1A804tight thermal1.140.5
2B804tight thermal1.130.5
3C804tight thermal2.020.5
1A4745medium thermal1.642
2B4745medium thermal1.342
3C4745medium thermal2.492
1A974loose thermal1.1210
2B974loose thermal1.0210
3C974loose thermal1.5910
LS refinement shellResolution: 2.7→2.769 Å / Total num. of bins used: 20
RfactorNum. reflection% reflection
Rfree0.294 142 -
Rwork0.242 5667 -
obs--100 %
Refinement TLS params.

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

IDL112)L122)L132)L222)L232)L332)S11 (Å °)S12 (Å °)S13 (Å °)S21 (Å °)S22 (Å °)S23 (Å °)S31 (Å °)S32 (Å °)S33 (Å °)T112)T122)T132)T222)T232)T332)Origin x (Å)Origin y (Å)Origin z (Å)
10.4601-0.1098-0.13360.84090.01350.4858-0.0218-0.0185-0.0274-0.0510.0369-0.09950.0482-0.0768-0.01510.2073-0.04570.01140.1147-0.0030.15634.806441.2732281.7285
21.9108-0.5536-0.30060.2813-0.07760.7216-0.018-0.0383-0.0271-0.11590.0037-0.0270.1422-0.15850.01430.2573-0.05-0.04460.13610.00480.091117.088547.4123268.2628
30.61490.66530.31560.75540.30781.8629-0.083-0.02980.078-0.1526-0.01380.1542-0.0742-0.27330.09680.1201-0.0554-0.13250.2180.02240.1578-0.839352.9384278.9338
40.40730.0691-0.03210.2501-0.00780.15-0.0095-0.05930.0213-0.0334-0.00170.0170.0108-0.04310.01110.1727-0.0482-0.02310.15830.00070.151317.664656.5259290.6037
50.375-0.0841-0.0081.3510.3610.7103-0.05440.0270.0725-0.09340.06150.07580.0139-0.0249-0.00710.1555-0.0135-0.03720.13510.02810.156716.03170.3716284.8764
60.8254-0.6703-0.08190.57520.07850.69810.1218-0.03160.1289-0.1574-0.0351-0.0682-0.0341-0.0534-0.08680.16680.0423-0.07130.1240.02090.206713.951984.1251278.5567
70.59750.0493-0.35410.5623-0.32350.48590.057-0.0353-0.01810.02870.00030.0171-0.0108-0.0253-0.05730.1478-0.0561-0.00890.19230.0150.152614.926438.1485336.6849
80.8857-0.50170.16750.3311-0.13840.07520.0312-0.2157-0.0303-0.00730.0190.0334-0.00910.034-0.05020.1577-0.0606-0.03440.26490.03780.1231.646533.5224346.1621
90.49540.21050.23430.6845-0.92882.15040.073-0.1281-0.0889-0.0291-0.10580.01510.20550.21580.03280.14950.0298-0.04080.15640.12720.165343.967413.3958335.0992
100.6197-0.37840.06310.8612-0.06470.01480.0307-0.023-0.0573-0.1459-0.01130.04030.038-0.0265-0.01940.1994-0.0573-0.03130.13210.03450.15626.631724.8155321.0956
110.2140.1445-0.1560.5271-0.02480.15680.0108-0.03080.00820.0047-0.0532-0.06320.01010.03710.04240.1663-0.0261-0.02150.16430.04460.16640.687734.5359326.7321
120.65290.8308-0.48151.3123-0.51291.643-0.00720.0747-0.1569-0.08990.0271-0.14940.16990.0707-0.01990.14340.04110.00960.12580.04730.216453.43832.1019312.1698
133.9057-0.4868-0.37140.3905-0.45460.80150.0812-0.2668-0.1152-0.0603-0.08660.02160.04310.19920.00550.11890.035-0.02020.18820.10480.180162.95636.2757324.5918
1413.6961-4.66160.93971.6176-0.46731.10690.17580.19080.2117-0.0948-0.1326-0.0808-0.07230.1609-0.04320.1740.03460.03360.1280.08130.196358.682746.1828313.5811
150.02610.1425-0.01121.39080.37450.54740.025-0.0053-0.00550.0353-0.08910.0085-0.02510.05940.06420.1845-0.0791-0.02130.13340.0120.16786.118924.4201306.3053
160.30220.1906-0.4160.38370.38812.2576-0.07120.0380.1579-0.10280.03750.21110.0091-0.130.03380.1554-0.062-0.05750.13110.06050.1638-2.401324.2213283.3352
170.27550.3298-0.02990.441-0.23151.1658-0.0981-0.0414-0.0692-0.1199-0.0271-0.0919-0.01390.09880.12520.2033-0.04980.03540.12730.03840.160517.117215.5915287.8153
180.15930.30810.01080.64250.01670.07-0.0652-0.00890.0405-0.15170.03040.02020.1139-0.03730.03480.2591-0.07570.00970.0991-0.00210.16172.26174.12283.0561
190.02710.12110.03631.1701-0.34240.9906-0.0762-0.02230.0224-0.4756-0.05670.07080.26260.02640.13290.4775-0.0679-0.03790.09250.01450.0456-7.2948-10.2051275.0656
Refinement TLS group
IDRefine-IDRefine TLS-IDAuth asym-IDAuth seq-ID
1X-RAY DIFFRACTION1A2 - 116
2X-RAY DIFFRACTION2A117 - 147
3X-RAY DIFFRACTION3A148 - 183
4X-RAY DIFFRACTION4A184 - 380
5X-RAY DIFFRACTION5A381 - 451
6X-RAY DIFFRACTION6A452 - 509
7X-RAY DIFFRACTION7B2 - 95
8X-RAY DIFFRACTION8B96 - 147
9X-RAY DIFFRACTION9B148 - 183
10X-RAY DIFFRACTION10B184 - 288
11X-RAY DIFFRACTION11B289 - 415
12X-RAY DIFFRACTION12B416 - 451
13X-RAY DIFFRACTION13B452 - 485
14X-RAY DIFFRACTION14B486 - 509
15X-RAY DIFFRACTION15C2 - 95
16X-RAY DIFFRACTION16C96 - 184
17X-RAY DIFFRACTION17C185 - 288
18X-RAY DIFFRACTION18C289 - 451
19X-RAY DIFFRACTION19C452 - 509

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