data_30545 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Structure of the Huttingtin tetramer/dimer mixture determined by paramagnetic NMR ; _BMRB_accession_number 30545 _BMRB_flat_file_name bmr30545.str _Entry_type original _Submission_date 2018-11-29 _Accession_date 2018-11-29 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Schwieters C. D. . 2 Kotler S. A. . 3 Schmidt T. . . 4 Ceccon A. . . 5 Ghirlando R. . . 6 Libich D. S. . 7 Clore G. M. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "13C chemical shifts" 21 "15N chemical shifts" 16 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-07-09 update BMRB 'update entry citation' 2019-02-08 original author 'original release' stop_ _Original_release_date 2018-12-05 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Probing initial transient oligomerization events facilitating Huntingtin fibril nucleation at atomic resolution by relaxation-based NMR ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 30808748 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Kotler S. A. . 2 Tugarinov V. . . 3 Schmidt T. . . 4 Ceccon A. . . 5 Libich D. S. . 6 Ghirlando R. . . 7 Schwieters C. D. . 8 Clore G. M. . stop_ _Journal_abbreviation 'Proc. Natl. Acad. Sci. U.S.A.' _Journal_name_full 'Proceedings of the National Academy of Sciences of the United States of America' _Journal_volume 116 _Journal_issue 9 _Journal_ISSN 1091-6490 _Journal_CSD 0353 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 3562 _Page_last 3571 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Huntingtin _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'entity_1, 1' $entity_1 'entity_1, 2' $entity_1 'entity_1, 3' $entity_1 'entity_1, 4' $entity_1 stop_ _System_molecular_weight . _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 2743.116 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 23 _Mol_residue_sequence ; ATLEKLMKAFESLKSFQQQQ QQQ ; loop_ _Residue_seq_code _Residue_label 1 ALA 2 THR 3 LEU 4 GLU 5 LYS 6 LEU 7 MET 8 LYS 9 ALA 10 PHE 11 GLU 12 SER 13 LEU 14 LYS 15 SER 16 PHE 17 GLN 18 GLN 19 GLN 20 GLN 21 GLN 22 GLN 23 GLN stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Gene_mnemonic $entity_1 Human 9606 Eukaryota Metazoa Homo sapiens 'HTT, HD, IT15' stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $entity_1 'recombinant technology' . Escherichia coli . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_2 _Saveframe_category sample _Sample_type solution _Details '1 mM [U-13C; U-15N] httNT-Q7, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1 mM '[U-13C; U-15N]' stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type solution _Details '1 mM 2-13C glucose; U-15N httNT-Q7, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1 mM [U-15N] stop_ save_ save_sample_4 _Saveframe_category sample _Sample_type solution _Details '0.6 mM [U-15N] httNT-Q7, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.6 mM [U-15N] stop_ save_ save_sample_5 _Saveframe_category sample _Sample_type solution _Details '0.75 mM 2-13C glucose; U-15N httNT-Q7, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.75 mM [U-15N] stop_ save_ save_sample_6 _Saveframe_category sample _Sample_type solution _Details '0.4 mM 2-13C glucose; U-15N httNT-Q7, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.4 mM [U-15N] stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name Xplor-NIH _Version 2.49 loop_ _Vendor _Address _Electronic_address 'C.D. Schwieters, J.J. Kuszewski, N. Tjandra, and G.M. Clore' . . stop_ loop_ _Task 'structure calculation' stop_ _Details . save_ save_software_2 _Saveframe_category software _Name Analysis _Version 2.4 loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_software_3 _Saveframe_category software _Name NMRDraw _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task 'peak picking' stop_ _Details . save_ save_software_4 _Saveframe_category software _Name NMRPipe _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task 'data analysis' processing stop_ _Details . save_ save_software_5 _Saveframe_category software _Name TOPSPIN _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceIII _Field_strength 600 _Details . save_ save_NMR_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceIII _Field_strength 800 _Details . save_ save_NMR_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceIII _Field_strength 900 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_2 save_ save_2D_1H-13C_CT_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C CT HSQC' _Sample_label $sample_2 save_ save_3D_CBCA(CO)NH_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCA(CO)NH' _Sample_label $sample_2 save_ save_3D_HNCACB_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCACB' _Sample_label $sample_2 save_ save_3D_TOCSY-HSQC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D TOCSY-HSQC' _Sample_label $sample_4 save_ save_13CA_SQ_CPMG_6 _Saveframe_category NMR_applied_experiment _Experiment_name '13CA SQ CPMG' _Sample_label $sample_3 save_ save_13CA_SQ_CPMG_7 _Saveframe_category NMR_applied_experiment _Experiment_name '13CA SQ CPMG' _Sample_label $sample_5 save_ save_15N_SQ_CPMG_8 _Saveframe_category NMR_applied_experiment _Experiment_name '15N SQ CPMG' _Sample_label $sample_3 save_ save_15N_SQ_CPMG_9 _Saveframe_category NMR_applied_experiment _Experiment_name '15N SQ CPMG' _Sample_label $sample_5 save_ save_1HN_PRE_10 _Saveframe_category NMR_applied_experiment _Experiment_name '1HN PRE' _Sample_label $sample_4 save_ save_13CA_SQ_CPMG_11 _Saveframe_category NMR_applied_experiment _Experiment_name '13CA SQ CPMG' _Sample_label $sample_6 save_ save_15N_SQ_CPMG_12 _Saveframe_category NMR_applied_experiment _Experiment_name '15N SQ CPMG' _Sample_label $sample_6 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 50 . mM pH 6.5 . pH pressure 1 . atm temperature 278 . K stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 50 . mM pH 6.5 . pH pressure 1 . atm temperature 283 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_shift_reference_1 _Saveframe_category chemical_shift_reference _Details . loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio DSS C 13 'methyl protons' ppm 0.000 internal indirect . . . 0.25144953 DSS H 1 'methyl protons' ppm 0.000 internal direct . . . 1.0 DSS N 15 'methyl protons' ppm 0.000 internal indirect . . . 0.10132912 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chemical_shifts_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-13C CT HSQC' '3D CBCA(CO)NH' '3D HNCACB' '3D TOCSY-HSQC' '13CA SQ CPMG' '15N SQ CPMG' '1HN PRE' stop_ loop_ _Sample_label $sample_2 $sample_4 $sample_3 $sample_5 $sample_6 stop_ _Sample_conditions_label $sample_conditions_2 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name 'entity_1, 1' _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 3 3 LEU CA C 57.849 0.310 1 2 3 3 LEU N N 122.695 0.430 1 3 4 4 GLU CA C 60.385 0.190 1 4 4 4 GLU N N 118.330 0.390 1 5 5 5 LYS CA C 59.476 0.140 1 6 5 5 LYS N N 119.959 0.190 1 7 6 6 LEU CA C 58.510 0.560 1 8 6 6 LEU N N 121.945 0.370 1 9 7 7 MET CA C 58.103 0.310 1 10 8 8 LYS CA C 59.042 0.130 1 11 8 8 LYS N N 119.674 0.210 1 12 9 9 ALA CA C 55.134 0.090 1 13 9 9 ALA N N 123.040 0.380 1 14 10 10 PHE CA C 60.896 0.150 1 15 10 10 PHE N N 119.002 0.350 1 16 11 11 GLU CA C 59.574 0.180 1 17 12 12 SER CA C 60.839 0.090 1 18 12 12 SER N N 114.563 0.390 1 19 13 13 LEU CA C 58.189 0.110 1 20 13 13 LEU N N 122.925 0.360 1 21 14 14 LYS CA C 58.805 0.100 1 22 14 14 LYS N N 119.848 0.370 1 23 15 15 SER CA C 60.844 0.090 1 24 15 15 SER N N 114.147 0.390 1 25 16 16 PHE CA C 59.857 0.080 1 26 17 17 GLN CA C 57.800 0.130 1 27 17 17 GLN N N 119.005 0.390 1 28 18 18 GLN CA C 56.643 0.140 1 29 18 18 GLN N N 119.250 0.380 1 30 19 19 GLN CA C 57.188 0.150 1 31 19 19 GLN N N 119.402 0.380 1 32 20 20 GLN CA C 56.089 0.140 1 33 20 20 GLN N N 119.368 0.380 1 34 21 21 GLN CA C 55.859 0.140 1 35 22 22 GLN CA C 55.885 0.140 1 36 22 22 GLN N N 121.794 0.360 1 37 23 23 GLN CA C 57.140 0.140 1 stop_ save_