data_36024 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR structure of TIBA, a chimera of SFTI ; _BMRB_accession_number 36024 _BMRB_flat_file_name bmr36024.str _Entry_type original _Submission_date 2016-10-10 _Accession_date 2016-06-11 _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 Xiao T. . . 2 Tam J. P. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 101 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-07-31 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 36023 'NMR structure of SLBA, a chimera of SFTI' stop_ _Original_release_date 2017-06-11 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; An Orally Active Bradykinin B1 Receptor Antagonist Engineered as a Bifunctional Chimera of Sunflower Trypsin Inhibitor. ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 27977181 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Qiu Y. . . 2 Taichi M. . . 3 Wei N. . . 4 Yang H. . . 5 Luo K. Q. . 6 Tam J. P. . stop_ _Journal_abbreviation 'J. Med. Chem.' _Journal_name_full 'Journal of medicinal chemistry' _Journal_volume 60 _Journal_issue 1 _Journal_ASTM JMCMAR _Journal_ISSN 1520-4804 _Journal_CSD 0151 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 504 _Page_last 510 _Year 2017 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Bradykinin-trypsin inhibitor secondary loop chimera' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity_1 $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 'Bradykinin-trypsin inhibitor secondary loop chimera' _Molecular_mass 1944.387 _Mol_thiol_state 'all disulfide bound' _Details 'cyclic peptide of DALK(BA) (RESIDUES 1-10) and TI loop SFTI (RESIDUES 11-18)' ############################## # Polymer residue sequence # ############################## _Residue_count 18 _Mol_residue_sequence ; CKRPPGFSPLCTKSIPPI ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 CYS 2 2 LYS 3 3 ARG 4 4 PRO 5 5 PRO 6 6 GLY 7 7 PHE 8 8 SER 9 9 PRO 10 10 LEU 11 11 CYS 12 12 THR 13 13 LYS 14 14 SER 15 15 ILE 16 16 PRO 17 17 PRO 18 18 ILE 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 $entity_1 'Helianthus annuus' 4232 Eukaryota Metazoa Helianthus annuus 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 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '1.3 mM NA TIBA, 0.01 % NA TFA, 55.56 M NA H2O, 1 mM NA sodium chloride, 95% H2O/5% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.3 mM 'natural abundance' TFA 0.01 % 'natural abundance' 'sodium chloride' 1 mM 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % [U-2H] stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name CNS _Version . loop_ _Task refinement stop_ _Details . save_ save_software_2 _Saveframe_category software _Name NMRPipe _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task processing stop_ _Details . save_ save_software_3 _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceII _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 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' 1 . mM pH 3.5 . pH pressure 1 . atm temperature 298 . 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 H 1 'methyl protons' ppm 0 external indirect . . . 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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-1H TOCSY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name entity_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 1 1 CYS H H 8.952 0.010 1 2 1 1 CYS HA H 5.536 0.003 1 3 1 1 CYS HB2 H 3.058 0.003 . 4 1 1 CYS HB3 H 2.731 0.005 . 5 2 2 LYS H H 8.741 0.002 1 6 2 2 LYS HA H 4.504 0.000 1 7 2 2 LYS HB2 H 1.818 0.000 . 8 2 2 LYS HB3 H 1.757 0.004 . 9 2 2 LYS HG2 H 1.418 0.004 . 10 2 2 LYS HD2 H 1.648 0.000 . 11 2 2 LYS HE2 H 2.913 0.000 . 12 3 3 ARG H H 8.706 0.007 1 13 3 3 ARG HA H 4.317 0.000 1 14 3 3 ARG HB2 H 1.819 0.000 . 15 3 3 ARG HB3 H 1.609 0.001 . 16 3 3 ARG HG2 H 1.430 0.000 . 17 3 3 ARG HD2 H 3.202 0.000 . 18 3 3 ARG HD3 H 3.166 0.000 . 19 3 3 ARG HE H 7.324 0.000 1 20 4 4 PRO HA H 4.462 0.005 1 21 4 4 PRO HB2 H 2.016 0.000 . 22 4 4 PRO HG2 H 1.679 0.001 . 23 4 4 PRO HD2 H 3.007 0.000 . 24 5 5 PRO HA H 4.340 0.001 1 25 5 5 PRO HB2 H 2.287 0.008 . 26 5 5 PRO HB3 H 2.157 0.006 . 27 5 5 PRO HG2 H 2.046 0.002 . 28 5 5 PRO HG3 H 1.928 0.000 . 29 5 5 PRO HD2 H 3.901 0.004 . 30 5 5 PRO HD3 H 3.674 0.014 . 31 6 6 GLY H H 8.626 0.011 1 32 6 6 GLY HA2 H 4.002 0.002 . 33 6 6 GLY HA3 H 3.562 0.001 . 34 7 7 PHE H H 7.861 0.008 1 35 7 7 PHE HA H 4.816 0.000 1 36 7 7 PHE HB2 H 3.353 0.003 . 37 7 7 PHE HB3 H 2.767 0.002 . 38 8 8 SER H H 8.449 0.001 1 39 8 8 SER HA H 4.713 0.003 1 40 8 8 SER HB2 H 3.960 0.005 . 41 8 8 SER HB3 H 3.862 0.003 . 42 9 9 PRO HA H 4.588 0.004 1 43 9 9 PRO HB2 H 2.291 0.000 . 44 9 9 PRO HG2 H 1.940 0.000 . 45 9 9 PRO HD2 H 3.815 0.001 . 46 9 9 PRO HD3 H 3.711 0.000 . 47 10 10 LEU H H 8.569 0.006 1 48 10 10 LEU HA H 4.656 0.000 1 49 10 10 LEU HB2 H 1.635 0.004 . 50 10 10 LEU HB3 H 1.635 0.004 . 51 10 10 LEU HG H 1.635 0.004 1 52 10 10 LEU HD1 H 0.889 0.000 . 53 10 10 LEU HD2 H 0.889 0.000 . 54 11 11 CYS H H 8.855 0.007 1 55 11 11 CYS HA H 5.633 0.003 1 56 11 11 CYS HB2 H 3.073 0.002 . 57 11 11 CYS HB3 H 2.978 0.003 . 58 12 12 THR H H 8.609 0.003 1 59 12 12 THR HA H 4.546 0.002 1 60 12 12 THR HB H 4.398 0.000 1 61 12 12 THR HG2 H 1.382 0.002 1 62 13 13 LYS H H 8.485 0.002 1 63 13 13 LYS HA H 4.472 0.004 1 64 13 13 LYS HB2 H 2.012 0.003 . 65 13 13 LYS HB3 H 1.683 0.000 . 66 13 13 LYS HG2 H 1.490 0.006 . 67 13 13 LYS HG3 H 1.406 0.004 . 68 13 13 LYS HD2 H 1.822 0.000 . 69 13 13 LYS HE2 H 3.006 0.000 . 70 14 14 SER H H 7.323 0.002 1 71 14 14 SER HA H 4.378 0.002 1 72 14 14 SER HB2 H 3.885 0.004 . 73 14 14 SER HB3 H 3.780 0.002 . 74 15 15 ILE H H 8.237 0.007 1 75 15 15 ILE HA H 4.282 0.006 1 76 15 15 ILE HB H 1.790 0.001 1 77 15 15 ILE HG12 H 1.448 0.003 . 78 15 15 ILE HG13 H 1.448 0.003 . 79 15 15 ILE HG2 H 1.043 0.001 1 80 15 15 ILE HD1 H 0.839 0.003 1 81 16 16 PRO HA H 5.085 0.002 1 82 16 16 PRO HB2 H 2.448 0.002 . 83 16 16 PRO HB3 H 2.024 0.002 . 84 16 16 PRO HG2 H 1.951 0.000 . 85 16 16 PRO HG3 H 1.849 0.003 . 86 16 16 PRO HD2 H 3.607 0.009 . 87 16 16 PRO HD3 H 3.524 0.006 . 88 17 17 PRO HA H 4.228 0.002 1 89 17 17 PRO HB2 H 2.421 0.003 . 90 17 17 PRO HB3 H 2.110 0.001 . 91 17 17 PRO HG2 H 1.867 0.003 . 92 17 17 PRO HG3 H 1.867 0.003 . 93 17 17 PRO HD2 H 3.801 0.002 . 94 17 17 PRO HD3 H 3.696 0.002 . 95 18 18 ILE H H 7.864 0.007 1 96 18 18 ILE HA H 4.319 0.000 1 97 18 18 ILE HB H 1.925 0.002 1 98 18 18 ILE HG12 H 1.450 0.002 . 99 18 18 ILE HG13 H 1.450 0.002 . 100 18 18 ILE HG2 H 1.148 0.001 1 101 18 18 ILE HD1 H 0.803 0.000 1 stop_ save_