data_53495 ####################### # Entry information # ####################### save_entry_information_1 _Entry.Sf_category entry_information _Entry.Sf_framecode entry_information_1 _Entry.ID 53495 _Entry.Title ; Chemical shift assignment of L50 in the free state at pH 7.2 ; _Entry.Type macromolecule _Entry.Version_type original _Entry.Submission_date 2025-12-27 _Entry.Accession_date 2025-12-27 _Entry.Last_release_date 2025-12-27 _Entry.Original_release_date 2025-12-27 _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 solution _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 'Chemical shift assignment of L50 in the free state at pH 7.2 determined by the 1H-1H and 1H-13C correlation experiments.' _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 Yuhei Nishimura . . . 0009-0009-0500-0505 53495 2 Yuji Tokunaga . . . 0000-0002-8774-9780 53495 3 Koh Takeuchi . . . 0000-0002-6227-4627 53495 stop_ loop_ _Entry_src.ID _Entry_src.Project_name _Entry_src.Organization_full_name _Entry_src.Organization_initials _Entry_src.Entry_ID 1 . 'Laboratory of Physical Chemistry, UT' . 53495 stop_ loop_ _Data_set.Type _Data_set.Count _Data_set.Entry_ID assigned_chemical_shifts 1 53495 stop_ loop_ _Datum.Type _Datum.Count _Datum.Entry_ID '13C chemical shifts' 22 53495 '1H chemical shifts' 44 53495 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 . . 2026-07-29 . original BMRB . 53495 stop_ loop_ _Related_entries.Database_name _Related_entries.Database_accession_code _Related_entries.Relationship _Related_entries.Entry_ID BMRB 53494 'Chemical shift assignment of L50 in the free state at pH 6.5' 53495 BMRB 53496 'Chemical shift assignment of L50 in the free state at pH 5.2' 53495 BMRB 53497 'Chemical shift assignment of L50 in the pre-miR-21-bound state at pH 5.2' 53495 BMRB 53498 'Chemical shift assignment of L50 in the pre-miR-21-bound state at pH 7.2' 53495 stop_ save_ ############### # Citations # ############### save_citations_1 _Citation.Sf_category citations _Citation.Sf_framecode citations_1 _Citation.Entry_ID 53495 _Citation.ID 1 _Citation.Name . _Citation.Class 'entry citation' _Citation.CAS_abstract_code . _Citation.MEDLINE_UI_code . _Citation.PubMed_ID 42467802 _Citation.DOI . _Citation.Full_citation . _Citation.Title ; Pre-miR-21 Conformational Equilibrium Modulates the Efficacy of the Maturation Inhibitor L50 ; _Citation.Status published _Citation.Type journal _Citation.Journal_abbrev 'ACS Chem. Biol.' _Citation.Journal_name_full 'ACS chemical biology' _Citation.Journal_volume . _Citation.Journal_issue . _Citation.Journal_ASTM . _Citation.Journal_ISSN 1554-8937 _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 . _Citation.Page_last . _Citation.Year 2026 _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 Yuhei Nishimura Y. . . . 53495 1 2 Yuji Tokunaga Y. . . . 53495 1 3 Yutaka Kofuku Y. . . . 53495 1 4 Yutaro Shiraishi Y. . . . 53495 1 5 Shunsuke Imai S. . . . 53495 1 6 Jing Gong J. . . . 53495 1 7 Kazuhiro Ohara K. . . . 53495 1 8 Junya Okude J. . . . 53495 1 9 Takumi Ueda T. . . . 53495 1 10 Takuya Torizawa T. . . . 53495 1 11 Ichio Shimada I. . . . 53495 1 12 Koh Takeuchi K. . . . 53495 1 stop_ save_ ############################################# # Molecular system (assembly) description # ############################################# save_assembly_1 _Assembly.Sf_category assembly _Assembly.Sf_framecode assembly_1 _Assembly.Entry_ID 53495 _Assembly.ID 1 _Assembly.Name L50 _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 . _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 L50 1 $entity_1 . . yes native no no . . . 53495 1 stop_ loop_ _Bond.ID _Bond.Type _Bond.Value_order _Bond.Assembly_atom_ID_1 _Bond.Entity_assembly_ID_1 _Bond.Entity_assembly_name_1 _Bond.Entity_ID_1 _Bond.Comp_ID_1 _Bond.Comp_index_ID_1 _Bond.Seq_ID_1 _Bond.Atom_ID_1 _Bond.Assembly_atom_ID_2 _Bond.Entity_assembly_ID_2 _Bond.Entity_assembly_name_2 _Bond.Entity_ID_2 _Bond.Comp_ID_2 _Bond.Comp_index_ID_2 _Bond.Seq_ID_2 _Bond.Atom_ID_2 _Bond.Auth_entity_assembly_ID_1 _Bond.Auth_entity_assembly_name_1 _Bond.Auth_asym_ID_1 _Bond.Auth_seq_ID_1 _Bond.Auth_comp_ID_1 _Bond.Auth_atom_ID_1 _Bond.Auth_entity_assembly_ID_2 _Bond.Auth_entity_assembly_name_2 _Bond.Auth_asym_ID_2 _Bond.Auth_seq_ID_2 _Bond.Auth_comp_ID_2 _Bond.Auth_atom_ID_2 _Bond.Entry_ID _Bond.Assembly_ID 1 peptide single . 1 . 1 ARG 1 1 N . 1 . 1 PRO 14 14 C . . . . . . . . . . . . 53495 1 stop_ save_ #################################### # Biological polymers and ligands # #################################### save_entity_1 _Entity.Sf_category entity _Entity.Sf_framecode entity_1 _Entity.Entry_ID 53495 _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 ; RVRTRGKRRIRRXP ; _Entity.Target_identifier . _Entity.Polymer_author_defined_seq . _Entity.Polymer_author_seq_details 'Residues 13 is D-Pro.' _Entity.Ambiguous_conformational_states no _Entity.Ambiguous_chem_comp_sites no _Entity.Nstd_monomer no _Entity.Nstd_chirality yes _Entity.Nstd_linkage no _Entity.Nonpolymer_comp_ID . _Entity.Nonpolymer_comp_label . _Entity.Number_of_monomers 14 _Entity.Number_of_nonpolymer_components . _Entity.Paramagnetic no _Entity.Thiol_state 'not present' _Entity.Src_method . _Entity.Parent_entity_ID 1 _Entity.Fragment . _Entity.Mutation . _Entity.EC_number . _Entity.Calc_isoelectric_point . _Entity.Formula_weight . _Entity.Formula_weight_exptl . _Entity.Formula_weight_exptl_meth . _Entity.Details 'The peptide was cyclized by a peptide bond between the first Arg and the last Pro.' _Entity.DB_query_date . _Entity.DB_query_revised_last_date . loop_ _Entity_biological_function.Biological_function _Entity_biological_function.Entry_ID _Entity_biological_function.Entity_ID 'pre-miR-21 maturation inihibitor' 53495 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 . ARG . 53495 1 2 . VAL . 53495 1 3 . ARG . 53495 1 4 . THR . 53495 1 5 . ARG . 53495 1 6 . GLY . 53495 1 7 . LYS . 53495 1 8 . ARG . 53495 1 9 . ARG . 53495 1 10 . ILE . 53495 1 11 . ARG . 53495 1 12 . ARG . 53495 1 13 . DPR . 53495 1 14 . PRO . 53495 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 . ARG 1 1 53495 1 . VAL 2 2 53495 1 . ARG 3 3 53495 1 . THR 4 4 53495 1 . ARG 5 5 53495 1 . GLY 6 6 53495 1 . LYS 7 7 53495 1 . ARG 8 8 53495 1 . ARG 9 9 53495 1 . ILE 10 10 53495 1 . ARG 11 11 53495 1 . ARG 12 12 53495 1 . DPR 13 13 53495 1 . PRO 14 14 53495 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 53495 _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 . . 'no natural source' . . . . . . . . . . . . . . . . . . . . . . 53495 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 53495 _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 . 'chemical synthesis' . . . . . . . . . . . . . . . . 53495 1 stop_ save_ ################################# # Polymer residues and ligands # ################################# save_chem_comp_DPR _Chem_comp.Sf_category chem_comp _Chem_comp.Sf_framecode chem_comp_DPR _Chem_comp.Entry_ID 53495 _Chem_comp.ID DPR _Chem_comp.Provenance PDB _Chem_comp.Name D-PROLINE _Chem_comp.Type 'D-PEPTIDE LINKING' _Chem_comp.BMRB_code DPR _Chem_comp.PDB_code DPR _Chem_comp.Ambiguous_flag no _Chem_comp.Initial_date 2020-07-10 _Chem_comp.Modified_date 2020-07-10 _Chem_comp.Release_status REL _Chem_comp.Replaced_by . _Chem_comp.Replaces . _Chem_comp.One_letter_code P _Chem_comp.Three_letter_code DPR _Chem_comp.Number_atoms_all 17 _Chem_comp.Number_atoms_nh 8 _Chem_comp.Atom_nomenclature_source . _Chem_comp.PubChem_code . _Chem_comp.Subcomponent_list . _Chem_comp.InChI_code InChI=1S/C5H9NO2/c7-5(8)4-2-1-3-6-4/h4,6H,1-3H2,(H,7,8)/t4-/m1/s1 _Chem_comp.Mon_nstd_flag no _Chem_comp.Mon_nstd_class . _Chem_comp.Mon_nstd_details . _Chem_comp.Mon_nstd_parent . _Chem_comp.Mon_nstd_parent_comp_ID . _Chem_comp.Std_deriv_one_letter_code . _Chem_comp.Std_deriv_three_letter_code . _Chem_comp.Std_deriv_BMRB_code . _Chem_comp.Std_deriv_PDB_code . _Chem_comp.Std_deriv_chem_comp_name . _Chem_comp.Synonyms . _Chem_comp.Formal_charge 0 _Chem_comp.Paramagnetic . _Chem_comp.Aromatic no _Chem_comp.Formula 'C5 H9 N O2' _Chem_comp.Formula_weight 115.130 _Chem_comp.Formula_mono_iso_wt_nat . _Chem_comp.Formula_mono_iso_wt_13C . _Chem_comp.Formula_mono_iso_wt_15N . _Chem_comp.Formula_mono_iso_wt_13C_15N . _Chem_comp.Image_file_name . _Chem_comp.Image_file_format . _Chem_comp.Topo_file_name . _Chem_comp.Topo_file_format . _Chem_comp.Struct_file_name . _Chem_comp.Struct_file_format . _Chem_comp.Stereochem_param_file_name . _Chem_comp.Stereochem_param_file_format . _Chem_comp.Model_details . _Chem_comp.Model_erf . _Chem_comp.Model_source . _Chem_comp.Model_coordinates_details . _Chem_comp.Model_coordinates_missing_flag yes _Chem_comp.Ideal_coordinates_details Corina _Chem_comp.Ideal_coordinates_missing_flag no _Chem_comp.Model_coordinates_db_code . _Chem_comp.Processing_site EBI _Chem_comp.Vendor . _Chem_comp.Vendor_product_code . _Chem_comp.Details . _Chem_comp.DB_query_date . _Chem_comp.DB_last_query_revised_last_date . loop_ _Chem_comp_descriptor.Descriptor _Chem_comp_descriptor.Type _Chem_comp_descriptor.Program _Chem_comp_descriptor.Program_version _Chem_comp_descriptor.Entry_ID _Chem_comp_descriptor.Comp_ID C1CC(NC1)C(=O)O SMILES 'OpenEye OEToolkits' 1.7.0 53495 DPR C1C[C@@H](NC1)C(=O)O SMILES_CANONICAL 'OpenEye OEToolkits' 1.7.0 53495 DPR InChI=1S/C5H9NO2/c7-5(8)4-2-1-3-6-4/h4,6H,1-3H2,(H,7,8)/t4-/m1/s1 InChI InChI 1.03 53495 DPR O=C(O)C1NCCC1 SMILES ACDLabs 12.01 53495 DPR OC(=O)[C@H]1CCCN1 SMILES_CANONICAL CACTVS 3.370 53495 DPR OC(=O)[CH]1CCCN1 SMILES CACTVS 3.370 53495 DPR ONIBWKKTOPOVIA-SCSAIBSYSA-N InChIKey InChI 1.03 53495 DPR stop_ loop_ _Chem_comp_identifier.Identifier _Chem_comp_identifier.Type _Chem_comp_identifier.Program _Chem_comp_identifier.Program_version _Chem_comp_identifier.Entry_ID _Chem_comp_identifier.Comp_ID '(2R)-pyrrolidine-2-carboxylic acid' 'SYSTEMATIC NAME' 'OpenEye OEToolkits' 1.7.0 53495 DPR D-proline 'SYSTEMATIC NAME' ACDLabs 12.01 53495 DPR stop_ loop_ _Chem_comp_atom.Atom_ID _Chem_comp_atom.BMRB_code _Chem_comp_atom.PDB_atom_ID _Chem_comp_atom.Alt_atom_ID _Chem_comp_atom.Auth_atom_ID _Chem_comp_atom.Type_symbol _Chem_comp_atom.Isotope_number _Chem_comp_atom.Chirality _Chem_comp_atom.Stereo_config _Chem_comp_atom.Charge _Chem_comp_atom.Partial_charge _Chem_comp_atom.Oxidation_number _Chem_comp_atom.Unpaired_electron_number _Chem_comp_atom.Align _Chem_comp_atom.Aromatic_flag _Chem_comp_atom.Leaving_atom_flag _Chem_comp_atom.Substruct_code _Chem_comp_atom.Ionizable _Chem_comp_atom.Drawing_2D_coord_x _Chem_comp_atom.Drawing_2D_coord_y _Chem_comp_atom.Model_Cartn_x _Chem_comp_atom.Model_Cartn_x_esd _Chem_comp_atom.Model_Cartn_y _Chem_comp_atom.Model_Cartn_y_esd _Chem_comp_atom.Model_Cartn_z _Chem_comp_atom.Model_Cartn_z_esd _Chem_comp_atom.Model_Cartn_x_ideal _Chem_comp_atom.Model_Cartn_y_ideal _Chem_comp_atom.Model_Cartn_z_ideal _Chem_comp_atom.PDBX_ordinal _Chem_comp_atom.Details _Chem_comp_atom.Entry_ID _Chem_comp_atom.Comp_ID N N N N . N . . N 0 . . . 1 N N . . . . -4.206 . 7.451 . -17.843 . 0.814 0.974 0.670 1 . 53495 DPR CA CA CA CA . C . . R 0 . . . 1 N N . . . . -3.893 . 8.671 . -18.566 . -0.014 -0.244 0.598 2 . 53495 DPR CB CB CB CB . C . . N 0 . . . 1 N N . . . . -5.242 . 9.255 . -18.952 . 0.728 -1.247 -0.310 3 . 53495 DPR CG CG CG CG . C . . N 0 . . . 1 N N . . . . -6.239 . 8.113 . -18.840 . 2.199 -0.759 -0.242 4 . 53495 DPR CD CD CD CD . C . . N 0 . . . 1 N N . . . . -5.571 . 6.986 . -18.070 . 2.016 0.777 -0.168 5 . 53495 DPR C C C C . C . . N 0 . . . 1 N N . . . . -2.999 . 8.379 . -19.774 . -1.360 0.086 0.006 6 . 53495 DPR O O O O . O . . N 0 . . . 1 N N . . . . -3.431 . 7.734 . -20.727 . -1.509 1.105 -0.626 7 . 53495 DPR OXT OXT OXT OXT . O . . N 0 . . . 1 N Y . . . . . . . . . . -2.393 -0.753 0.180 8 . 53495 DPR H H H HT1 . H . . N 0 . . . 1 N Y . . . . -3.576 . 6.736 . -18.147 . 0.293 1.784 0.370 9 . 53495 DPR HA HA HA HA . H . . N 0 . . . 1 N N . . . . -3.318 . 9.388 . -17.962 . -0.138 -0.667 1.595 10 . 53495 DPR HB2 HB2 HB2 HB1 . H . . N 0 . . . 1 N N . . . . -5.517 . 10.078 . -18.276 . 0.639 -2.260 0.083 11 . 53495 DPR HB3 HB3 HB3 HB2 . H . . N 0 . . . 1 N N . . . . -5.215 . 9.648 . -19.979 . 0.351 -1.194 -1.331 12 . 53495 DPR HG2 HG2 HG2 HG1 . H . . N 0 . . . 1 N N . . . . -7.140 . 8.451 . -18.307 . 2.695 -1.137 0.653 13 . 53495 DPR HG3 HG3 HG3 HG2 . H . . N 0 . . . 1 N N . . . . -6.527 . 7.765 . -19.843 . 2.747 -1.045 -1.140 14 . 53495 DPR HD2 HD2 HD2 HD1 . H . . N 0 . . . 1 N N . . . . -5.580 . 6.051 . -18.650 . 1.855 1.188 -1.165 15 . 53495 DPR HD3 HD3 HD3 HD2 . H . . N 0 . . . 1 N N . . . . -6.088 . 6.796 . -17.118 . 2.885 1.241 0.299 16 . 53495 DPR HXT HXT HXT HXT . H . . N 0 . . . 1 N Y . . . . . . . . . . -3.237 -0.500 -0.219 17 . 53495 DPR stop_ loop_ _Chem_comp_bond.ID _Chem_comp_bond.Type _Chem_comp_bond.Value_order _Chem_comp_bond.Atom_ID_1 _Chem_comp_bond.Atom_ID_2 _Chem_comp_bond.Aromatic_flag _Chem_comp_bond.Stereo_config _Chem_comp_bond.Ordinal _Chem_comp_bond.Details _Chem_comp_bond.Entry_ID _Chem_comp_bond.Comp_ID 1 . SING N CA N N 1 . 53495 DPR 2 . SING N CD N N 2 . 53495 DPR 3 . SING N H N N 3 . 53495 DPR 4 . SING CA CB N N 4 . 53495 DPR 5 . SING CA C N N 5 . 53495 DPR 6 . SING CA HA N N 6 . 53495 DPR 7 . SING CB CG N N 7 . 53495 DPR 8 . SING CB HB2 N N 8 . 53495 DPR 9 . SING CB HB3 N N 9 . 53495 DPR 10 . SING CG CD N N 10 . 53495 DPR 11 . SING CG HG2 N N 11 . 53495 DPR 12 . SING CG HG3 N N 12 . 53495 DPR 13 . SING CD HD2 N N 13 . 53495 DPR 14 . SING CD HD3 N N 14 . 53495 DPR 15 . DOUB C O N N 15 . 53495 DPR 16 . SING C OXT N N 16 . 53495 DPR 17 . SING OXT HXT N N 17 . 53495 DPR stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Sample.Sf_category sample _Sample.Sf_framecode sample_1 _Sample.Entry_ID 53495 _Sample.ID 1 _Sample.Name 'L50 in D2O' _Sample.Type solution _Sample.Sub_type . _Sample.Details . _Sample.Aggregate_sample_number 1 _Sample.Solvent_system '100% D2O' _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 L50 'natural abundance' . . 1 $entity_1 . . 500 . . uM . . . . 53495 1 2 D2O 'natural abundance' . . . . . . 99.96 . . % . . . . 53495 1 3 TRIS '[U-99% 2H]' . . . . . . 20 . . mM . . . . 53495 1 4 'Malonic Acid' '[U-99% 2H]' . . . . . . 20 . . mM . . . . 53495 1 5 EDTA 'natural abundance' . . . . . . 0.01 . . mM . . . . 53495 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 53495 _Sample_condition_list.ID 1 _Sample_condition_list.Name '99.96 % D2O' _Sample_condition_list.Details ; 500 uM peptide was dissolved in 20 mM Tris-Malonate buffer (pH 7.2), containing 20 mM NaCl, and supplemented with 100% D2O. ; 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 'ionic strength' 0.02 . M 53495 1 pH 7.2 . pH 53495 1 pressure 1 . atm 53495 1 temperature 310 . K 53495 1 stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Software.Sf_category software _Software.Sf_framecode software_1 _Software.Entry_ID 53495 _Software.ID 1 _Software.Type . _Software.Name NMRFAM-SPARKY _Software.Version . _Software.DOI . _Software.Details . loop_ _Task.Task _Task.Software_module _Task.Entry_ID _Task.Software_ID 'chemical shift assignment' . 53495 1 'chemical shift calculation' . 53495 1 'data analysis' . 53495 1 stop_ save_ save_software_2 _Software.Sf_category software _Software.Sf_framecode software_2 _Software.Entry_ID 53495 _Software.ID 2 _Software.Type . _Software.Name TOPSPIN _Software.Version . _Software.DOI . _Software.Details . loop_ _Task.Task _Task.Software_module _Task.Entry_ID _Task.Software_ID collection . 53495 2 processing . 53495 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 53495 _NMR_spectrometer.ID 1 _NMR_spectrometer.Name 'Bruker AVANCE III HD 800MHz' _NMR_spectrometer.Details . _NMR_spectrometer.Manufacturer Bruker _NMR_spectrometer.Model 'AVANCE III HD' _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 53495 _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 1H-13C HSQC' no no no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 1 $NMR_spectrometer_1 . . . . . . . . . . . . . . . . . 53495 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 53495 _Chem_shift_reference.ID 1 _Chem_shift_reference.Name DSS-310K _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 DSS 'methyl protons' . . . . ppm 0.00 external indirect 0.251449530 . . . . . 53495 1 H 1 DSS 'methyl protons' . . . . ppm 0.00 external direct 1.000000000 . . . . . 53495 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 53495 _Assigned_chem_shift_list.ID 1 _Assigned_chem_shift_list.Name L50-free-pH72_310K _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 . _Assigned_chem_shift_list.Chem_shift_15N_err . _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 1H-13C HSQC' . . . 53495 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 . . 53495 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 2 2 VAL HB H 1 1.93 0.01 . 1 . . . . . 2 VAL HB . 53495 1 2 . 1 . 1 2 2 VAL HG11 H 1 0.87 0.01 . 2 . . . . . 2 VAL HG11 . 53495 1 3 . 1 . 1 2 2 VAL HG12 H 1 0.87 0.01 . 2 . . . . . 2 VAL HG12 . 53495 1 4 . 1 . 1 2 2 VAL HG13 H 1 0.87 0.01 . 2 . . . . . 2 VAL HG13 . 53495 1 5 . 1 . 1 2 2 VAL HG21 H 1 0.82 0.01 . 2 . . . . . 2 VAL HG21 . 53495 1 6 . 1 . 1 2 2 VAL HG22 H 1 0.82 0.01 . 2 . . . . . 2 VAL HG22 . 53495 1 7 . 1 . 1 2 2 VAL HG23 H 1 0.82 0.01 . 2 . . . . . 2 VAL HG23 . 53495 1 8 . 1 . 1 2 2 VAL CB C 13 33.8 0.2 . 1 . . . . . 2 VAL CB . 53495 1 9 . 1 . 1 2 2 VAL CG1 C 13 21.0 0.2 . 2 . . . . . 2 VAL CG1 . 53495 1 10 . 1 . 1 2 2 VAL CG2 C 13 21.3 0.2 . 2 . . . . . 2 VAL CG2 . 53495 1 11 . 1 . 1 4 4 THR HB H 1 4.08 0.01 . 1 . . . . . 4 THR HB . 53495 1 12 . 1 . 1 4 4 THR HG21 H 1 1.11 0.01 . 1 . . . . . 4 THR HG21 . 53495 1 13 . 1 . 1 4 4 THR HG22 H 1 1.11 0.01 . 1 . . . . . 4 THR HG22 . 53495 1 14 . 1 . 1 4 4 THR HG23 H 1 1.11 0.01 . 1 . . . . . 4 THR HG23 . 53495 1 15 . 1 . 1 4 4 THR CB C 13 69.9 0.2 . 1 . . . . . 4 THR CB . 53495 1 16 . 1 . 1 4 4 THR CG2 C 13 21.8 0.2 . 1 . . . . . 4 THR CG2 . 53495 1 17 . 1 . 1 6 6 GLY HA2 H 1 3.73 0.01 . 2 . . . . . 6 GLY HA2 . 53495 1 18 . 1 . 1 6 6 GLY HA3 H 1 4.05 0.01 . 2 . . . . . 6 GLY HA3 . 53495 1 19 . 1 . 1 6 6 GLY CA C 13 46.7 0.2 . 1 . . . . . 6 GLY CA . 53495 1 20 . 1 . 1 7 7 LYS HA H 1 4.25 0.01 . 1 . . . . . 7 LYS HA . 53495 1 21 . 1 . 1 7 7 LYS HB2 H 1 2.01 0.01 . 1 . . . . . 7 LYS HB2 . 53495 1 22 . 1 . 1 7 7 LYS HB3 H 1 2.01 0.01 . 1 . . . . . 7 LYS HB3 . 53495 1 23 . 1 . 1 7 7 LYS HG2 H 1 1.47 0.01 . 1 . . . . . 7 LYS HG2 . 53495 1 24 . 1 . 1 7 7 LYS HG3 H 1 1.47 0.01 . 1 . . . . . 7 LYS HG3 . 53495 1 25 . 1 . 1 7 7 LYS HD2 H 1 1.70 0.01 . 1 . . . . . 7 LYS HD2 . 53495 1 26 . 1 . 1 7 7 LYS HD3 H 1 1.70 0.01 . 1 . . . . . 7 LYS HD3 . 53495 1 27 . 1 . 1 7 7 LYS HE2 H 1 3.01 0.01 . 1 . . . . . 7 LYS HE2 . 53495 1 28 . 1 . 1 7 7 LYS HE3 H 1 3.01 0.01 . 1 . . . . . 7 LYS HE3 . 53495 1 29 . 1 . 1 7 7 LYS CA C 13 56.6 0.2 . 1 . . . . . 7 LYS CA . 53495 1 30 . 1 . 1 7 7 LYS CB C 13 32.5 0.2 . 1 . . . . . 7 LYS CB . 53495 1 31 . 1 . 1 7 7 LYS CG C 13 25.1 0.2 . 1 . . . . . 7 LYS CG . 53495 1 32 . 1 . 1 7 7 LYS CD C 13 28.9 0.2 . 1 . . . . . 7 LYS CD . 53495 1 33 . 1 . 1 7 7 LYS CE C 13 41.9 0.2 . 1 . . . . . 7 LYS CE . 53495 1 34 . 1 . 1 10 10 ILE HA H 1 4.35 0.01 . 1 . . . . . 10 ILE HA . 53495 1 35 . 1 . 1 10 10 ILE HB H 1 1.80 0.01 . 1 . . . . . 10 ILE HB . 53495 1 36 . 1 . 1 10 10 ILE HG12 H 1 1.11 0.01 . 2 . . . . . 10 ILE HG12 . 53495 1 37 . 1 . 1 10 10 ILE HG13 H 1 1.38 0.01 . 2 . . . . . 10 ILE HG13 . 53495 1 38 . 1 . 1 10 10 ILE HG21 H 1 0.87 0.01 . 1 . . . . . 10 ILE HG21 . 53495 1 39 . 1 . 1 10 10 ILE HG22 H 1 0.87 0.01 . 1 . . . . . 10 ILE HG22 . 53495 1 40 . 1 . 1 10 10 ILE HG23 H 1 0.87 0.01 . 1 . . . . . 10 ILE HG23 . 53495 1 41 . 1 . 1 10 10 ILE HD11 H 1 0.80 0.01 . 1 . . . . . 10 ILE HD11 . 53495 1 42 . 1 . 1 10 10 ILE HD12 H 1 0.80 0.01 . 1 . . . . . 10 ILE HD12 . 53495 1 43 . 1 . 1 10 10 ILE HD13 H 1 0.80 0.01 . 1 . . . . . 10 ILE HD13 . 53495 1 44 . 1 . 1 10 10 ILE CA C 13 60.0 0.2 . 1 . . . . . 10 ILE CA . 53495 1 45 . 1 . 1 10 10 ILE CB C 13 40.3 0.2 . 1 . . . . . 10 ILE CB . 53495 1 46 . 1 . 1 10 10 ILE CG1 C 13 27.3 0.2 . 1 . . . . . 10 ILE CG1 . 53495 1 47 . 1 . 1 10 10 ILE CG2 C 13 17.7 0.2 . 1 . . . . . 10 ILE CG2 . 53495 1 48 . 1 . 1 10 10 ILE CD1 C 13 13.4 0.2 . 1 . . . . . 10 ILE CD . 53495 1 49 . 1 . 1 13 13 DPR HB2 H 1 1.93 0.01 . 2 . . . . . 13 DPR HB2 . 53495 1 50 . 1 . 1 13 13 DPR HB3 H 1 2.31 0.01 . 2 . . . . . 13 DPR HB3 . 53495 1 51 . 1 . 1 13 13 DPR HG2 H 1 2.14 0.01 . 2 . . . . . 13 DPR HG2 . 53495 1 52 . 1 . 1 13 13 DPR HG3 H 1 2.03 0.01 . 2 . . . . . 13 DPR HG3 . 53495 1 53 . 1 . 1 13 13 DPR HD2 H 1 3.82 0.01 . 2 . . . . . 13 DPR HD2 . 53495 1 54 . 1 . 1 13 13 DPR HD3 H 1 3.51 0.01 . 2 . . . . . 13 DPR HD3 . 53495 1 55 . 1 . 1 13 13 DPR CB C 13 30.6 0.2 . 1 . . . . . 13 DPR CB . 53495 1 56 . 1 . 1 13 13 DPR CG C 13 27.7 0.2 . 1 . . . . . 13 DPR CG . 53495 1 57 . 1 . 1 13 13 DPR CD C 13 51.0 0.2 . 1 . . . . . 13 DPR CD . 53495 1 58 . 1 . 1 14 14 PRO HB2 H 1 2.27 0.01 . 2 . . . . . 14 PRO HB2 . 53495 1 59 . 1 . 1 14 14 PRO HB3 H 1 2.11 0.01 . 2 . . . . . 14 PRO HB3 . 53495 1 60 . 1 . 1 14 14 PRO HG2 H 1 1.92 0.01 . 2 . . . . . 14 PRO HG2 . 53495 1 61 . 1 . 1 14 14 PRO HG3 H 1 2.11 0.01 . 2 . . . . . 14 PRO HG3 . 53495 1 62 . 1 . 1 14 14 PRO HD2 H 1 3.75 0.01 . 2 . . . . . 14 PRO HD2 . 53495 1 63 . 1 . 1 14 14 PRO HD3 H 1 3.98 0.01 . 2 . . . . . 14 PRO HD3 . 53495 1 64 . 1 . 1 14 14 PRO CB C 13 32.4 0.2 . 1 . . . . . 14 PRO CB . 53495 1 65 . 1 . 1 14 14 PRO CG C 13 26.5 0.2 . 1 . . . . . 14 PRO CG . 53495 1 66 . 1 . 1 14 14 PRO CD C 13 51.0 0.2 . 1 . . . . . 14 PRO CD . 53495 1 stop_ save_