data_51584 ####################### # Entry information # ####################### save_entry_information_1 _Entry.Sf_category entry_information _Entry.Sf_framecode entry_information_1 _Entry.ID 51584 _Entry.Title ; Backbone 13C and 15N Chemical Shift Assignments for fibrillar Amyloid Beta (1-42) at pH 7.0 ; _Entry.Type macromolecule _Entry.Version_type original _Entry.Submission_date 2022-08-18 _Entry.Accession_date 2022-08-18 _Entry.Last_release_date 2022-08-18 _Entry.Original_release_date 2022-08-18 _Entry.Origination author _Entry.Format_name . _Entry.NMR_STAR_version 3.2.14.0 _Entry.NMR_STAR_dict_location . _Entry.Original_NMR_STAR_version 3.1 _Entry.Experimental_method NMR _Entry.Experimental_method_subtype solid-state _Entry.Source_data_format . _Entry.Source_data_format_version . _Entry.Generated_software_name . _Entry.Generated_software_version . _Entry.Generated_software_ID . _Entry.Generated_software_label . _Entry.Generated_date . _Entry.DOI . _Entry.UUID . _Entry.Related_coordinate_file_name . _Entry.Details . _Entry.BMRB_internal_directory_name . loop_ _Entry_author.Ordinal _Entry_author.Given_name _Entry_author.Family_name _Entry_author.First_initial _Entry_author.Middle_initials _Entry_author.Family_title _Entry_author.ORCID _Entry_author.Entry_ID 1 Nina Becker . . . 0000-0002-6617-2775 51584 2 Luis Gardon . . . 0000-0003-0871-6487 51584 3 Lothar Gremer . . . 0000-0001-7065-5027 51584 4 Dieter Willbold . . . 0000-0002-0065-7366 51584 5 Henrike Heise . . . 0000-0002-9081-3894 51584 stop_ loop_ _Entry_src.ID _Entry_src.Project_name _Entry_src.Organization_full_name _Entry_src.Organization_initials _Entry_src.Entry_ID 1 . 'Institut fuer Physikalische Biologie, Heinrich-Heine Universitaet Dusseldorf' . 51584 2 . 'IBI-7 (Strukturbiochemie), Forschungszentrum Juelich' . 51584 stop_ loop_ _Data_set.Type _Data_set.Count _Data_set.Entry_ID assigned_chemical_shifts 1 51584 stop_ loop_ _Datum.Type _Datum.Count _Datum.Entry_ID '13C chemical shifts' 52 51584 '15N chemical shifts' 21 51584 stop_ loop_ _Release.Release_number _Release.Format_type _Release.Format_version _Release.Date _Release.Submission_date _Release.Type _Release.Author _Release.Detail _Release.Entry_ID 1 . . 2023-05-10 . original BMRB . 51584 stop_ loop_ _Related_entries.Database_name _Related_entries.Database_accession_code _Related_entries.Relationship _Related_entries.Entry_ID BMRB 27212 'Backbone 13C and 15N Chemical Shift Assignments for fibrillar Amyloid Beta (1-42) at pH 2.0' 51584 BMRB 51321 'Sequence-specific Backbone Resonance Assignments of Human Amyloid-beta(1-42) in 28% Acetonitrile at pH 2.0' 51584 BMRB 51322 'Sequence-specific Backbone Resonance Assignments of Human Amyloid-beta(1-42) at pH 7.0' 51584 BMRB 51323 'Sequence-specific Backbone Resonance Assignments of Human Amyloid-beta(1-42) at pH 2.0' 51584 PDB 5OQV 'Near-atomic resolution fibril structure of complete amyloid-beta(1-42) by cryo-EM' 51584 stop_ save_ ############### # Citations # ############### save_citations_1 _Citation.Sf_category citations _Citation.Sf_framecode citations_1 _Citation.Entry_ID 51584 _Citation.ID 1 _Citation.Name . _Citation.Class 'entry citation' _Citation.CAS_abstract_code . _Citation.MEDLINE_UI_code . _Citation.PubMed_ID 36653015 _Citation.DOI . _Citation.Full_citation . _Citation.Title ; Atomic Resolution Insights into pH Shift Induced Deprotonation Events in LS-Shaped Ab(1-42) Amyloid Fibrils ; _Citation.Status published _Citation.Type journal _Citation.Journal_abbrev 'J. Am. Chem. Soc.' _Citation.Journal_name_full 'Journal of the American Chemical Society' _Citation.Journal_volume 145 _Citation.Journal_issue 4 _Citation.Journal_ASTM . _Citation.Journal_ISSN 1520-5126 _Citation.Journal_CSD . _Citation.Book_title . _Citation.Book_chapter_title . _Citation.Book_volume . _Citation.Book_series . _Citation.Book_publisher . _Citation.Book_publisher_city . _Citation.Book_ISBN . _Citation.Conference_title . _Citation.Conference_site . _Citation.Conference_state_province . _Citation.Conference_country . _Citation.Conference_start_date . _Citation.Conference_end_date . _Citation.Conference_abstract_number . _Citation.Thesis_institution . _Citation.Thesis_institution_city . _Citation.Thesis_institution_country . _Citation.WWW_URL . _Citation.Page_first 2161 _Citation.Page_last 2169 _Citation.Year 2023 _Citation.Details . loop_ _Citation_author.Ordinal _Citation_author.Given_name _Citation_author.Family_name _Citation_author.First_initial _Citation_author.Middle_initials _Citation_author.Family_title _Citation_author.ORCID _Citation_author.Entry_ID _Citation_author.Citation_ID 1 Nina Becker . . . . 51584 1 2 Benedikt Frieg . . . . 51584 1 3 Lothar Gremer . . . . 51584 1 4 Tatsiana Kupreichyk . . . . 51584 1 5 Patrick Freiburg . . . . 51584 1 6 Luis Gardon . . . . 51584 1 7 Philipp Neudecker . . . . 51584 1 8 Dieter Willbold . . . . 51584 1 9 Holger Gohlke . . . . 51584 1 10 Henrike Heise . . . . 51584 1 stop_ save_ ############################################# # Molecular system (assembly) description # ############################################# save_assembly_1 _Assembly.Sf_category assembly _Assembly.Sf_framecode assembly_1 _Assembly.Entry_ID 51584 _Assembly.ID 1 _Assembly.Name 'amyloid beta(1-42)' _Assembly.BMRB_code . _Assembly.Number_of_components 1 _Assembly.Organic_ligands 0 _Assembly.Metal_ions 0 _Assembly.Non_standard_bonds no _Assembly.Ambiguous_conformational_states no _Assembly.Ambiguous_chem_comp_sites . _Assembly.Molecules_in_chemical_exchange no _Assembly.Paramagnetic no _Assembly.Thiol_state . _Assembly.Molecular_mass 4514.1 _Assembly.Enzyme_commission_number . _Assembly.Details . _Assembly.DB_query_date . _Assembly.DB_query_revised_last_date . loop_ _Entity_assembly.ID _Entity_assembly.Entity_assembly_name _Entity_assembly.Entity_ID _Entity_assembly.Entity_label _Entity_assembly.Asym_ID _Entity_assembly.PDB_chain_ID _Entity_assembly.Experimental_data_reported _Entity_assembly.Physical_state _Entity_assembly.Conformational_isomer _Entity_assembly.Chemical_exchange_state _Entity_assembly.Magnetic_equivalence_group_code _Entity_assembly.Role _Entity_assembly.Details _Entity_assembly.Entry_ID _Entity_assembly.Assembly_ID 1 Abeta(1-42) 1 $entity_1 . . yes fibril no no . . . 51584 1 stop_ save_ #################################### # Biological polymers and ligands # #################################### save_entity_1 _Entity.Sf_category entity _Entity.Sf_framecode entity_1 _Entity.Entry_ID 51584 _Entity.ID 1 _Entity.BMRB_code . _Entity.Name entity_1 _Entity.Type polymer _Entity.Polymer_common_type . _Entity.Polymer_type polypeptide(L) _Entity.Polymer_type_details . _Entity.Polymer_strand_ID . _Entity.Polymer_seq_one_letter_code_can . _Entity.Polymer_seq_one_letter_code ; DAEFRHDSGYEVHHQKLVFF AEDVGSNKGAIIGLMVGGVV IA ; _Entity.Target_identifier . _Entity.Polymer_author_defined_seq . _Entity.Polymer_author_seq_details . _Entity.Ambiguous_conformational_states no _Entity.Ambiguous_chem_comp_sites no _Entity.Nstd_monomer no _Entity.Nstd_chirality no _Entity.Nstd_linkage no _Entity.Nonpolymer_comp_ID . _Entity.Nonpolymer_comp_label . _Entity.Number_of_monomers 42 _Entity.Number_of_nonpolymer_components . _Entity.Paramagnetic no _Entity.Thiol_state 'not present' _Entity.Src_method . _Entity.Parent_entity_ID 1 _Entity.Fragment 'Amyloid-beta protein 42 (672-713)' _Entity.Mutation . _Entity.EC_number . _Entity.Calc_isoelectric_point . _Entity.Formula_weight 4514.1 _Entity.Formula_weight_exptl . _Entity.Formula_weight_exptl_meth . _Entity.Details . _Entity.DB_query_date . _Entity.DB_query_revised_last_date . loop_ _Entity_db_link.Ordinal _Entity_db_link.Author_supplied _Entity_db_link.Database_code _Entity_db_link.Accession_code _Entity_db_link.Entry_mol_code _Entity_db_link.Entry_mol_name _Entity_db_link.Entry_experimental_method _Entity_db_link.Entry_structure_resolution _Entity_db_link.Entry_relation_type _Entity_db_link.Entry_details _Entity_db_link.Chimera_segment_ID _Entity_db_link.Seq_query_to_submitted_percent _Entity_db_link.Seq_subject_length _Entity_db_link.Seq_identity _Entity_db_link.Seq_positive _Entity_db_link.Seq_homology_expectation_val _Entity_db_link.Seq_align_begin _Entity_db_link.Seq_align_end _Entity_db_link.Seq_difference_details _Entity_db_link.Seq_alignment_details _Entity_db_link.Entry_ID _Entity_db_link.Entity_ID 1 yes UNP P05067 . APP . . . . . . . . . . . . . . 51584 1 stop_ loop_ _Entity_comp_index.ID _Entity_comp_index.Auth_seq_ID _Entity_comp_index.Comp_ID _Entity_comp_index.Comp_label _Entity_comp_index.Entry_ID _Entity_comp_index.Entity_ID 1 . ASP . 51584 1 2 . ALA . 51584 1 3 . GLU . 51584 1 4 . PHE . 51584 1 5 . ARG . 51584 1 6 . HIS . 51584 1 7 . ASP . 51584 1 8 . SER . 51584 1 9 . GLY . 51584 1 10 . TYR . 51584 1 11 . GLU . 51584 1 12 . VAL . 51584 1 13 . HIS . 51584 1 14 . HIS . 51584 1 15 . GLN . 51584 1 16 . LYS . 51584 1 17 . LEU . 51584 1 18 . VAL . 51584 1 19 . PHE . 51584 1 20 . PHE . 51584 1 21 . ALA . 51584 1 22 . GLU . 51584 1 23 . ASP . 51584 1 24 . VAL . 51584 1 25 . GLY . 51584 1 26 . SER . 51584 1 27 . ASN . 51584 1 28 . LYS . 51584 1 29 . GLY . 51584 1 30 . ALA . 51584 1 31 . ILE . 51584 1 32 . ILE . 51584 1 33 . GLY . 51584 1 34 . LEU . 51584 1 35 . MET . 51584 1 36 . VAL . 51584 1 37 . GLY . 51584 1 38 . GLY . 51584 1 39 . VAL . 51584 1 40 . VAL . 51584 1 41 . ILE . 51584 1 42 . ALA . 51584 1 stop_ loop_ _Entity_poly_seq.Hetero _Entity_poly_seq.Mon_ID _Entity_poly_seq.Num _Entity_poly_seq.Comp_index_ID _Entity_poly_seq.Entry_ID _Entity_poly_seq.Entity_ID . ASP 1 1 51584 1 . ALA 2 2 51584 1 . GLU 3 3 51584 1 . PHE 4 4 51584 1 . ARG 5 5 51584 1 . HIS 6 6 51584 1 . ASP 7 7 51584 1 . SER 8 8 51584 1 . GLY 9 9 51584 1 . TYR 10 10 51584 1 . GLU 11 11 51584 1 . VAL 12 12 51584 1 . HIS 13 13 51584 1 . HIS 14 14 51584 1 . GLN 15 15 51584 1 . LYS 16 16 51584 1 . LEU 17 17 51584 1 . VAL 18 18 51584 1 . PHE 19 19 51584 1 . PHE 20 20 51584 1 . ALA 21 21 51584 1 . GLU 22 22 51584 1 . ASP 23 23 51584 1 . VAL 24 24 51584 1 . GLY 25 25 51584 1 . SER 26 26 51584 1 . ASN 27 27 51584 1 . LYS 28 28 51584 1 . GLY 29 29 51584 1 . ALA 30 30 51584 1 . ILE 31 31 51584 1 . ILE 32 32 51584 1 . GLY 33 33 51584 1 . LEU 34 34 51584 1 . MET 35 35 51584 1 . VAL 36 36 51584 1 . GLY 37 37 51584 1 . GLY 38 38 51584 1 . VAL 39 39 51584 1 . VAL 40 40 51584 1 . ILE 41 41 51584 1 . ALA 42 42 51584 1 stop_ save_ #################### # Natural source # #################### save_natural_source_1 _Entity_natural_src_list.Sf_category natural_source _Entity_natural_src_list.Sf_framecode natural_source_1 _Entity_natural_src_list.Entry_ID 51584 _Entity_natural_src_list.ID 1 loop_ _Entity_natural_src.ID _Entity_natural_src.Entity_ID _Entity_natural_src.Entity_label _Entity_natural_src.Entity_chimera_segment_ID _Entity_natural_src.NCBI_taxonomy_ID _Entity_natural_src.Type _Entity_natural_src.Common _Entity_natural_src.Organism_name_scientific _Entity_natural_src.Organism_name_common _Entity_natural_src.Organism_acronym _Entity_natural_src.ICTVdb_decimal_code _Entity_natural_src.Superkingdom _Entity_natural_src.Kingdom _Entity_natural_src.Genus _Entity_natural_src.Species _Entity_natural_src.Strain _Entity_natural_src.Variant _Entity_natural_src.Organ _Entity_natural_src.Tissue _Entity_natural_src.Tissue_fraction _Entity_natural_src.Cell_line _Entity_natural_src.Cell_type _Entity_natural_src.ATCC_number _Entity_natural_src.Organelle _Entity_natural_src.Secretion _Entity_natural_src.Plasmid _Entity_natural_src.Gene_mnemonic _Entity_natural_src.Details _Entity_natural_src.Entry_ID _Entity_natural_src.Entity_natural_src_list_ID 1 1 $entity_1 . 9606 organism . 'Homo sapiens' Human . . Eukaryota Metazoa Homo sapiens . . . . . . . . . . . APP . 51584 1 stop_ save_ ######################### # Experimental source # ######################### save_experimental_source_1 _Entity_experimental_src_list.Sf_category experimental_source _Entity_experimental_src_list.Sf_framecode experimental_source_1 _Entity_experimental_src_list.Entry_ID 51584 _Entity_experimental_src_list.ID 1 loop_ _Entity_experimental_src.ID _Entity_experimental_src.Entity_ID _Entity_experimental_src.Entity_label _Entity_experimental_src.Entity_chimera_segment_ID _Entity_experimental_src.Production_method _Entity_experimental_src.Host_org_scientific_name _Entity_experimental_src.Host_org_name_common _Entity_experimental_src.Host_org_details _Entity_experimental_src.Host_org_NCBI_taxonomy_ID _Entity_experimental_src.Host_org_genus _Entity_experimental_src.Host_org_species _Entity_experimental_src.Host_org_strain _Entity_experimental_src.Host_org_variant _Entity_experimental_src.Host_org_ATCC_number _Entity_experimental_src.Vector_type _Entity_experimental_src.PDBview_host_org_vector_name _Entity_experimental_src.PDBview_plasmid_name _Entity_experimental_src.Vector_name _Entity_experimental_src.Vector_details _Entity_experimental_src.Vendor_name _Entity_experimental_src.Details _Entity_experimental_src.Entry_ID _Entity_experimental_src.Entity_experimental_src_list_ID 1 1 $entity_1 . 'recombinant technology' 'Escherichia coli' . . . Escherichia coli BL21(DE3) . . plasmid . . pET302/NT-His . . . 51584 1 stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Sample.Sf_category sample _Sample.Sf_framecode sample_1 _Sample.Entry_ID 51584 _Sample.ID 1 _Sample.Name 'LS-shaped amyloid beta (1-42) fibrils at pH 7.0' _Sample.Type fibrils _Sample.Sub_type . _Sample.Details . _Sample.Aggregate_sample_number 1 _Sample.Solvent_system '24% acetonitrile, 0.08% trifluoroacetic acid, 8.825 mM citric acid, 82.35 mM Na2HPO4, pH 7.0' _Sample.Preparation_date . _Sample.Preparation_expiration_date . _Sample.Polycrystallization_protocol . _Sample.Single_crystal_protocol . _Sample.Crystal_grow_apparatus . _Sample.Crystal_grow_atmosphere . _Sample.Crystal_grow_details . _Sample.Crystal_grow_method . _Sample.Crystal_grow_method_cit_ID . _Sample.Crystal_grow_pH . _Sample.Crystal_grow_pH_range . _Sample.Crystal_grow_pressure . _Sample.Crystal_grow_pressure_esd . _Sample.Crystal_grow_seeding . _Sample.Crystal_grow_seeding_cit_ID . _Sample.Crystal_grow_temp . _Sample.Crystal_grow_temp_details . _Sample.Crystal_grow_temp_esd . _Sample.Crystal_grow_time . _Sample.Oriented_sample_prep_protocol . _Sample.Lyophilization_cryo_protectant . _Sample.Storage_protocol . loop_ _Sample_component.ID _Sample_component.Mol_common_name _Sample_component.Isotopic_labeling _Sample_component.Assembly_ID _Sample_component.Assembly_label _Sample_component.Entity_ID _Sample_component.Entity_label _Sample_component.Product_ID _Sample_component.Type _Sample_component.Concentration_val _Sample_component.Concentration_val_min _Sample_component.Concentration_val_max _Sample_component.Concentration_val_units _Sample_component.Concentration_val_err _Sample_component.Vendor _Sample_component.Vendor_product_name _Sample_component.Vendor_product_code _Sample_component.Entry_ID _Sample_component.Sample_ID 1 Abeta(1-42) '[U-13C; U-15N]' . . 1 $entity_1 . . 1.5 1.0 2.0 mM . . . . 51584 1 2 acetonitrile 'natural abundance' . . . . . . 24 . . '% v/v' . . . . 51584 1 3 'trifluoroacetic acid' 'natural abundance' . . . . . . 0.08 . . '% v/v' . . . . 51584 1 4 'citric acid' 'natural abundance' . . . . . . 8.825 . . mM . . . . 51584 1 5 Na2HPO4 'natural abundance' . . . . . . 82.35 . . mM . . . . 51584 1 6 H2O 'natural abundance' . . . . . . 76 . . '% v/v' . . . . 51584 1 stop_ save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Sample_condition_list.Sf_category sample_conditions _Sample_condition_list.Sf_framecode sample_conditions_1 _Sample_condition_list.Entry_ID 51584 _Sample_condition_list.ID 1 _Sample_condition_list.Name 'LS-shaped amyloid beta (1-42) fibrils at pH 7.0' _Sample_condition_list.Details . loop_ _Sample_condition_variable.Type _Sample_condition_variable.Val _Sample_condition_variable.Val_err _Sample_condition_variable.Val_units _Sample_condition_variable.Entry_ID _Sample_condition_variable.Sample_condition_list_ID pH 7.0 0.1 pH 51584 1 pressure 1 . atm 51584 1 temperature 273 5 K 51584 1 stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Software.Sf_category software _Software.Sf_framecode software_1 _Software.Entry_ID 51584 _Software.ID 1 _Software.Type . _Software.Name CcpNMR _Software.Version 2.4.2 _Software.DOI . _Software.Details . loop_ _Task.Task _Task.Software_module _Task.Entry_ID _Task.Software_ID 'chemical shift assignment' . 51584 1 stop_ save_ save_software_2 _Software.Sf_category software _Software.Sf_framecode software_2 _Software.Entry_ID 51584 _Software.ID 2 _Software.Type . _Software.Name TOPSPIN _Software.Version '4.0.1; 3.5' _Software.DOI . _Software.Details . loop_ _Task.Task _Task.Software_module _Task.Entry_ID _Task.Software_ID collection . 51584 2 processing . 51584 2 stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _NMR_spectrometer.Sf_category NMR_spectrometer _NMR_spectrometer.Sf_framecode NMR_spectrometer_1 _NMR_spectrometer.Entry_ID 51584 _NMR_spectrometer.ID 1 _NMR_spectrometer.Name B600 _NMR_spectrometer.Details . _NMR_spectrometer.Manufacturer Bruker _NMR_spectrometer.Model 'AVANCE NEO' _NMR_spectrometer.Serial_number . _NMR_spectrometer.Field_strength 600 save_ save_NMR_spectrometer_2 _NMR_spectrometer.Sf_category NMR_spectrometer _NMR_spectrometer.Sf_framecode NMR_spectrometer_2 _NMR_spectrometer.Entry_ID 51584 _NMR_spectrometer.ID 2 _NMR_spectrometer.Name B800 _NMR_spectrometer.Details . _NMR_spectrometer.Manufacturer Bruker _NMR_spectrometer.Model 'AVANCE III' _NMR_spectrometer.Serial_number . _NMR_spectrometer.Field_strength 800 save_ ############################# # NMR applied experiments # ############################# save_experiment_list_1 _Experiment_list.Sf_category experiment_list _Experiment_list.Sf_framecode experiment_list_1 _Experiment_list.Entry_ID 51584 _Experiment_list.ID 1 _Experiment_list.Details . loop_ _Experiment.ID _Experiment.Name _Experiment.Raw_data_flag _Experiment.NUS_flag _Experiment.Interleaved_flag _Experiment.NMR_spec_expt_ID _Experiment.NMR_spec_expt_label _Experiment.MS_expt_ID _Experiment.MS_expt_label _Experiment.SAXS_expt_ID _Experiment.SAXS_expt_label _Experiment.FRET_expt_ID _Experiment.FRET_expt_label _Experiment.EMR_expt_ID _Experiment.EMR_expt_label _Experiment.Sample_ID _Experiment.Sample_label _Experiment.Sample_state _Experiment.Sample_volume _Experiment.Sample_volume_units _Experiment.Sample_condition_list_ID _Experiment.Sample_condition_list_label _Experiment.Sample_spinning_rate _Experiment.Sample_angle _Experiment.NMR_tube_type _Experiment.NMR_spectrometer_ID _Experiment.NMR_spectrometer_label _Experiment.NMR_spectrometer_probe_ID _Experiment.NMR_spectrometer_probe_label _Experiment.NMR_spectral_processing_ID _Experiment.NMR_spectral_processing_label _Experiment.Mass_spectrometer_ID _Experiment.Mass_spectrometer_label _Experiment.Xray_instrument_ID _Experiment.Xray_instrument_label _Experiment.Fluorescence_instrument_ID _Experiment.Fluorescence_instrument_label _Experiment.EMR_instrument_ID _Experiment.EMR_instrument_label _Experiment.Chromatographic_system_ID _Experiment.Chromatographic_system_label _Experiment.Chromatographic_column_ID _Experiment.Chromatographic_column_label _Experiment.Details _Experiment.Entry_ID _Experiment.Experiment_list_ID 1 '2D NCaCX' no no no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 1 $NMR_spectrometer_1 . . . . . . . . . . . . . . . . . 51584 1 2 '2D NCOCX' no no no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 1 $NMR_spectrometer_1 . . . . . . . . . . . . . . . . . 51584 1 3 '2D 13C-13C PDSD' no no no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 2 $NMR_spectrometer_2 . . . . . . . . . . . . . . . . . 51584 1 4 '2D NCa' no no no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 2 $NMR_spectrometer_2 . . . . . . . . . . . . . . . . . 51584 1 stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_shift_reference_1 _Chem_shift_reference.Sf_category chem_shift_reference _Chem_shift_reference.Sf_framecode chem_shift_reference_1 _Chem_shift_reference.Entry_ID 51584 _Chem_shift_reference.ID 1 _Chem_shift_reference.Name chem_shift_reference_1 _Chem_shift_reference.Details . loop_ _Chem_shift_ref.Atom_type _Chem_shift_ref.Atom_isotope_number _Chem_shift_ref.Mol_common_name _Chem_shift_ref.Atom_group _Chem_shift_ref.Concentration_val _Chem_shift_ref.Concentration_units _Chem_shift_ref.Solvent _Chem_shift_ref.Rank _Chem_shift_ref.Chem_shift_units _Chem_shift_ref.Chem_shift_val _Chem_shift_ref.Ref_method _Chem_shift_ref.Ref_type _Chem_shift_ref.Indirect_shift_ratio _Chem_shift_ref.External_ref_loc _Chem_shift_ref.External_ref_sample_geometry _Chem_shift_ref.External_ref_axis _Chem_shift_ref.Ref_correction_type _Chem_shift_ref.Correction_val _Chem_shift_ref.Entry_ID _Chem_shift_ref.Chem_shift_reference_ID C 13 adamantane 'methine carbon' . . . . ppm 31.4 external direct 1.0 'separate tube (no insert) similar to the experimental sample tube' . . . . 51584 1 N 15 'liquid anhydrous ammonia' nitrogen . . . . ppm 0 na direct 1.0 . . . . . 51584 1 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 _Assigned_chem_shift_list.Sf_category assigned_chemical_shifts _Assigned_chem_shift_list.Sf_framecode assigned_chemical_shifts_1 _Assigned_chem_shift_list.Entry_ID 51584 _Assigned_chem_shift_list.ID 1 _Assigned_chem_shift_list.Name assigned_chemical_shifts_1 _Assigned_chem_shift_list.Sample_condition_list_ID 1 _Assigned_chem_shift_list.Sample_condition_list_label $sample_conditions_1 _Assigned_chem_shift_list.Chem_shift_reference_ID 1 _Assigned_chem_shift_list.Chem_shift_reference_label $chem_shift_reference_1 _Assigned_chem_shift_list.Chem_shift_1H_err . _Assigned_chem_shift_list.Chem_shift_13C_err 0.5 _Assigned_chem_shift_list.Chem_shift_15N_err 1 _Assigned_chem_shift_list.Chem_shift_31P_err . _Assigned_chem_shift_list.Chem_shift_2H_err . _Assigned_chem_shift_list.Chem_shift_19F_err . _Assigned_chem_shift_list.Error_derivation_method . _Assigned_chem_shift_list.Details . _Assigned_chem_shift_list.Text_data_format . _Assigned_chem_shift_list.Text_data . loop_ _Chem_shift_experiment.Experiment_ID _Chem_shift_experiment.Experiment_name _Chem_shift_experiment.Sample_ID _Chem_shift_experiment.Sample_label _Chem_shift_experiment.Sample_state _Chem_shift_experiment.Entry_ID _Chem_shift_experiment.Assigned_chem_shift_list_ID 1 '2D NCaCX' . . . 51584 1 2 '2D NCOCX' . . . 51584 1 3 '2D 13C-13C PDSD' . . . 51584 1 4 '2D NCa' . . . 51584 1 stop_ loop_ _Chem_shift_software.Software_ID _Chem_shift_software.Software_label _Chem_shift_software.Method_ID _Chem_shift_software.Method_label _Chem_shift_software.Entry_ID _Chem_shift_software.Assigned_chem_shift_list_ID 1 $software_1 . . 51584 1 stop_ loop_ _Atom_chem_shift.ID _Atom_chem_shift.Assembly_atom_ID _Atom_chem_shift.Entity_assembly_ID _Atom_chem_shift.Entity_assembly_asym_ID _Atom_chem_shift.Entity_ID _Atom_chem_shift.Comp_index_ID _Atom_chem_shift.Seq_ID _Atom_chem_shift.Comp_ID _Atom_chem_shift.Atom_ID _Atom_chem_shift.Atom_type _Atom_chem_shift.Atom_isotope_number _Atom_chem_shift.Val _Atom_chem_shift.Val_err _Atom_chem_shift.Assign_fig_of_merit _Atom_chem_shift.Ambiguity_code _Atom_chem_shift.Ambiguity_set_ID _Atom_chem_shift.Occupancy _Atom_chem_shift.Resonance_ID _Atom_chem_shift.Auth_entity_assembly_ID _Atom_chem_shift.Auth_asym_ID _Atom_chem_shift.Auth_seq_ID _Atom_chem_shift.Auth_comp_ID _Atom_chem_shift.Auth_atom_ID _Atom_chem_shift.Details _Atom_chem_shift.Entry_ID _Atom_chem_shift.Assigned_chem_shift_list_ID 1 . 1 . 1 19 19 PHE CA C 13 56.5400 0.5 . 1 . . . . . 19 PHE CA . 51584 1 2 . 1 . 1 19 19 PHE N N 15 122.1150 1 . 1 . . . . . 19 PHE N . 51584 1 3 . 1 . 1 20 20 PHE CA C 13 56.3480 0.5 . 1 . . . . . 20 PHE CA . 51584 1 4 . 1 . 1 20 20 PHE CB C 13 43.0560 0.5 . 1 . . . . . 20 PHE CB . 51584 1 5 . 1 . 1 20 20 PHE N N 15 131.5170 1 . 1 . . . . . 20 PHE N . 51584 1 6 . 1 . 1 21 21 ALA CA C 13 49.0740 0.5 . 1 . . . . . 21 ALA CA . 51584 1 7 . 1 . 1 21 21 ALA CB C 13 22.4020 0.5 . 1 . . . . . 21 ALA CB . 51584 1 8 . 1 . 1 21 21 ALA N N 15 129.8590 1 . 1 . . . . . 21 ALA N . 51584 1 9 . 1 . 1 24 24 VAL CA C 13 58.0100 0.5 . 1 . . . . . 24 VAL CA . 51584 1 10 . 1 . 1 24 24 VAL CB C 13 36.1090 0.5 . 1 . . . . . 24 VAL CB . 51584 1 11 . 1 . 1 24 24 VAL CG1 C 13 21.1350 0.5 . 2 . . . . . 24 VAL CG1 . 51584 1 12 . 1 . 1 24 24 VAL CG2 C 13 23.0440 0.5 . 2 . . . . . 24 VAL CG2 . 51584 1 13 . 1 . 1 24 24 VAL N N 15 117.7680 1 . 1 . . . . . 24 VAL N . 51584 1 14 . 1 . 1 25 25 GLY CA C 13 48.7510 0.5 . 1 . . . . . 25 GLY CA . 51584 1 15 . 1 . 1 25 25 GLY N N 15 116.6310 1 . 1 . . . . . 25 GLY N . 51584 1 16 . 1 . 1 26 26 SER CA C 13 56.6300 0.5 . 1 . . . . . 26 SER CA . 51584 1 17 . 1 . 1 26 26 SER CB C 13 65.6390 0.5 . 1 . . . . . 26 SER CB . 51584 1 18 . 1 . 1 26 26 SER N N 15 113.1110 1 . 1 . . . . . 26 SER N . 51584 1 19 . 1 . 1 27 27 ASN CA C 13 52.3060 0.5 . 1 . . . . . 27 ASN CA . 51584 1 20 . 1 . 1 27 27 ASN CB C 13 40.9830 0.5 . 1 . . . . . 27 ASN CB . 51584 1 21 . 1 . 1 27 27 ASN N N 15 118.7430 1 . 1 . . . . . 27 ASN N . 51584 1 22 . 1 . 1 28 28 LYS CA C 13 54.9090 0.5 . 1 . . . . . 28 LYS CA . 51584 1 23 . 1 . 1 28 28 LYS CB C 13 35.3120 0.5 . 1 . . . . . 28 LYS CB . 51584 1 24 . 1 . 1 28 28 LYS CG C 13 25.4880 0.5 . 1 . . . . . 28 LYS CG . 51584 1 25 . 1 . 1 28 28 LYS CD C 13 29.9870 0.5 . 1 . . . . . 28 LYS CD . 51584 1 26 . 1 . 1 28 28 LYS CE C 13 42.7220 0.5 . 1 . . . . . 28 LYS CE . 51584 1 27 . 1 . 1 28 28 LYS N N 15 128.0600 1 . 1 . . . . . 28 LYS N . 51584 1 28 . 1 . 1 29 29 GLY CA C 13 44.6210 0.5 . 1 . . . . . 29 GLY CA . 51584 1 29 . 1 . 1 29 29 GLY N N 15 111.4570 1 . 1 . . . . . 29 GLY N . 51584 1 30 . 1 . 1 30 30 ALA CA C 13 49.0810 0.5 . 1 . . . . . 30 ALA CA . 51584 1 31 . 1 . 1 30 30 ALA CB C 13 22.1990 0.5 . 1 . . . . . 30 ALA CB . 51584 1 32 . 1 . 1 30 30 ALA N N 15 122.3310 1 . 1 . . . . . 30 ALA N . 51584 1 33 . 1 . 1 31 31 ILE CA C 13 59.9610 0.5 . 1 . . . . . 31 ILE CA . 51584 1 34 . 1 . 1 31 31 ILE CB C 13 40.4400 0.5 . 1 . . . . . 31 ILE CB . 51584 1 35 . 1 . 1 31 31 ILE CG1 C 13 27.2010 0.5 . 1 . . . . . 31 ILE CG1 . 51584 1 36 . 1 . 1 31 31 ILE CG2 C 13 17.6860 0.5 . 1 . . . . . 31 ILE CG2 . 51584 1 37 . 1 . 1 31 31 ILE CD1 C 13 14.3600 0.5 . 1 . . . . . 31 ILE CD1 . 51584 1 38 . 1 . 1 31 31 ILE N N 15 122.0730 1 . 1 . . . . . 31 ILE N . 51584 1 39 . 1 . 1 32 32 ILE CA C 13 57.5750 0.5 . 1 . . . . . 32 ILE CA . 51584 1 40 . 1 . 1 32 32 ILE CB C 13 42.8210 0.5 . 1 . . . . . 32 ILE CB . 51584 1 41 . 1 . 1 32 32 ILE CG1 C 13 26.7760 0.5 . 1 . . . . . 32 ILE CG1 . 51584 1 42 . 1 . 1 32 32 ILE CG2 C 13 18.2890 0.5 . 1 . . . . . 32 ILE CG2 . 51584 1 43 . 1 . 1 32 32 ILE CD1 C 13 16.1450 0.5 . 1 . . . . . 32 ILE CD1 . 51584 1 44 . 1 . 1 32 32 ILE N N 15 124.2170 1 . 1 . . . . . 32 ILE N . 51584 1 45 . 1 . 1 33 33 GLY N N 15 113.4480 1 . 1 . . . . . 33 GLY N . 51584 1 46 . 1 . 1 34 34 LEU CA C 13 54.3820 0.5 . 1 . . . . . 34 LEU CA . 51584 1 47 . 1 . 1 34 34 LEU CG C 13 27.9110 0.5 . 1 . . . . . 34 LEU CG . 51584 1 48 . 1 . 1 35 35 MET CA C 13 54.4150 0.5 . 1 . . . . . 35 MET CA . 51584 1 49 . 1 . 1 35 35 MET CG C 13 31.6620 0.5 . 1 . . . . . 35 MET CG . 51584 1 50 . 1 . 1 35 35 MET N N 15 126.9160 1 . 1 . . . . . 35 MET N . 51584 1 51 . 1 . 1 36 36 VAL CA C 13 61.4540 0.5 . 1 . . . . . 36 VAL CA . 51584 1 52 . 1 . 1 36 36 VAL CB C 13 33.7350 0.5 . 1 . . . . . 36 VAL CB . 51584 1 53 . 1 . 1 36 36 VAL N N 15 124.6450 1 . 1 . . . . . 36 VAL N . 51584 1 54 . 1 . 1 37 37 GLY C C 13 169.7440 0.5 . 1 . . . . . 37 GLY C . 51584 1 55 . 1 . 1 37 37 GLY CA C 13 45.0590 0.5 . 1 . . . . . 37 GLY CA . 51584 1 56 . 1 . 1 37 37 GLY N N 15 106.2250 1 . 1 . . . . . 37 GLY N . 51584 1 57 . 1 . 1 38 38 GLY C C 13 172.8760 0.5 . 1 . . . . . 38 GLY C . 51584 1 58 . 1 . 1 38 38 GLY CA C 13 43.7280 0.5 . 1 . . . . . 38 GLY CA . 51584 1 59 . 1 . 1 38 38 GLY N N 15 101.1830 1 . 1 . . . . . 38 GLY N . 51584 1 60 . 1 . 1 39 39 VAL CA C 13 60.5680 0.5 . 1 . . . . . 39 VAL CA . 51584 1 61 . 1 . 1 39 39 VAL CB C 13 36.5440 0.5 . 1 . . . . . 39 VAL CB . 51584 1 62 . 1 . 1 39 39 VAL CG1 C 13 21.0370 0.5 . 2 . . . . . 39 VAL CG1 . 51584 1 63 . 1 . 1 39 39 VAL N N 15 118.9130 1 . 1 . . . . . 39 VAL N . 51584 1 64 . 1 . 1 40 40 VAL CA C 13 60.2120 0.5 . 1 . . . . . 40 VAL CA . 51584 1 65 . 1 . 1 40 40 VAL CB C 13 34.8560 0.5 . 1 . . . . . 40 VAL CB . 51584 1 66 . 1 . 1 40 40 VAL N N 15 126.8530 1 . 1 . . . . . 40 VAL N . 51584 1 67 . 1 . 1 41 41 ILE CA C 13 59.6780 0.5 . 1 . . . . . 41 ILE CA . 51584 1 68 . 1 . 1 41 41 ILE CG1 C 13 26.9740 0.5 . 1 . . . . . 41 ILE CG1 . 51584 1 69 . 1 . 1 41 41 ILE N N 15 127.2530 1 . 1 . . . . . 41 ILE N . 51584 1 70 . 1 . 1 42 42 ALA C C 13 182.0560 0.5 . 1 . . . . . 42 ALA C . 51584 1 71 . 1 . 1 42 42 ALA CA C 13 53.4970 0.5 . 1 . . . . . 42 ALA CA . 51584 1 72 . 1 . 1 42 42 ALA CB C 13 19.6650 0.5 . 1 . . . . . 42 ALA CB . 51584 1 73 . 1 . 1 42 42 ALA N N 15 133.9860 1 . 1 . . . . . 42 ALA N . 51584 1 stop_ save_