data_36023 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR structure of SLBA, a chimera of SFTI ; _BMRB_accession_number 36023 _BMRB_flat_file_name bmr36023.str _Entry_type original _Submission_date 2016-10-10 _Accession_date 2017-06-11 _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" 79 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-07-31 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 36024 'NMR structure of TIBA, 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 1780.102 _Mol_thiol_state 'all disulfide bound' _Details 'cyclic peptide from SFTI (RESIDUES 1-6) and DALK(BA) (RESIDUES 7-16)' ############################## # Polymer residue sequence # ############################## _Residue_count 16 _Mol_residue_sequence ; CFPDGRCKRPPGFSPL ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 CYS 2 2 PHE 3 3 PRO 4 4 ASP 5 5 GLY 6 6 ARG 7 7 CYS 8 8 LYS 9 9 ARG 10 10 PRO 11 11 PRO 12 12 GLY 13 13 PHE 14 14 SER 15 15 PRO 16 16 LEU 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 '1.5 mM NA SLBA, 55.56 M NA H2O, 1 mM NA sodium chloride, 0.01 % NA TFA, 95% H2O/5% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.5 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_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _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 TOCSY' '2D 1H-1H NOESY' 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 8.488 0.002 1 2 1 1 CYS HA H 5.180 0.010 1 3 1 1 CYS HB2 H 2.952 0.001 . 4 1 1 CYS HB3 H 2.875 0.009 . 5 2 2 PHE H H 8.655 0.002 1 6 2 2 PHE HA H 4.894 0.000 1 7 2 2 PHE HB2 H 3.362 0.002 . 8 2 2 PHE HB3 H 3.039 0.002 . 9 2 2 PHE HD1 H 7.318 0.002 . 10 3 3 PRO HA H 4.409 0.001 1 11 3 3 PRO HB2 H 2.417 0.001 . 12 3 3 PRO HB3 H 2.173 0.000 . 13 3 3 PRO HG2 H 2.064 0.001 . 14 3 3 PRO HD2 H 4.027 0.002 . 15 3 3 PRO HD3 H 3.960 0.004 . 16 4 4 ASP H H 7.933 0.002 1 17 4 4 ASP HA H 4.557 0.002 1 18 4 4 ASP HB2 H 3.129 0.000 . 19 4 4 ASP HB3 H 2.823 0.000 . 20 5 5 GLY H H 8.412 0.002 1 21 5 5 GLY HA2 H 4.251 0.002 . 22 5 5 GLY HA3 H 3.799 0.002 . 23 6 6 ARG H H 7.847 0.002 1 24 6 6 ARG HA H 4.436 0.002 1 25 6 6 ARG HB2 H 1.965 0.005 . 26 6 6 ARG HB3 H 1.855 0.002 . 27 6 6 ARG HG2 H 1.593 0.005 . 28 6 6 ARG HD2 H 3.175 0.000 . 29 6 6 ARG HE H 7.417 0.002 1 30 7 7 CYS H H 8.562 0.007 1 31 7 7 CYS HA H 5.481 0.010 1 32 7 7 CYS HB2 H 3.098 0.013 . 33 7 7 CYS HB3 H 2.713 0.010 . 34 8 8 LYS H H 9.166 0.005 1 35 8 8 LYS HA H 4.529 0.000 1 36 8 8 LYS HB2 H 1.880 0.004 . 37 8 8 LYS HB3 H 1.831 0.000 . 38 8 8 LYS HG2 H 1.465 0.000 . 39 8 8 LYS HD2 H 1.723 0.000 . 40 8 8 LYS HE2 H 2.931 0.000 . 41 9 9 ARG H H 8.668 0.006 1 42 9 9 ARG HA H 4.217 0.000 1 43 9 9 ARG HB2 H 1.790 0.002 . 44 9 9 ARG HB3 H 1.615 0.003 . 45 9 9 ARG HG2 H 1.418 0.002 . 46 9 9 ARG HE H 7.281 0.000 1 47 10 10 PRO HA H 4.408 0.000 1 48 10 10 PRO HB2 H 2.386 0.000 . 49 10 10 PRO HB3 H 2.173 0.000 . 50 10 10 PRO HD2 H 3.957 0.000 . 51 10 10 PRO HD3 H 4.026 0.000 . 52 11 11 PRO HA H 4.351 0.001 1 53 11 11 PRO HB2 H 2.280 0.002 . 54 11 11 PRO HB3 H 2.166 0.000 . 55 11 11 PRO HG2 H 1.938 0.000 . 56 11 11 PRO HD2 H 3.915 0.000 . 57 12 12 GLY H H 8.640 0.001 1 58 12 12 GLY HA2 H 3.998 0.001 . 59 12 12 GLY HA3 H 3.559 0.000 . 60 13 13 PHE H H 7.807 0.006 1 61 13 13 PHE HA H 4.166 0.000 1 62 13 13 PHE HB2 H 3.322 0.004 . 63 13 13 PHE HB3 H 2.739 0.003 . 64 14 14 SER H H 8.488 0.001 1 65 14 14 SER HA H 4.694 0.002 1 66 14 14 SER HB2 H 3.926 0.000 . 67 14 14 SER HB3 H 3.836 0.002 . 68 15 15 PRO HA H 4.585 0.002 1 69 15 15 PRO HB2 H 2.146 0.001 . 70 15 15 PRO HB3 H 2.081 0.000 . 71 15 15 PRO HG2 H 1.952 0.001 . 72 15 15 PRO HG3 H 1.910 0.009 . 73 15 15 PRO HD2 H 3.803 0.001 . 74 15 15 PRO HD3 H 3.698 0.000 . 75 16 16 LEU H H 8.477 0.001 1 76 16 16 LEU HA H 4.505 0.005 1 77 16 16 LEU HB2 H 1.534 0.003 . 78 16 16 LEU HG H 1.412 0.000 1 79 16 16 LEU HD1 H 0.840 0.003 . stop_ save_