data_36016 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Structure of roseltide rT1 ; _BMRB_accession_number 36016 _BMRB_flat_file_name bmr36016.str _Entry_type original _Submission_date 2016-08-16 _Accession_date 2016-12-20 _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" 132 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-04-24 original BMRB . stop_ _Original_release_date 2016-12-20 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Identification and Characterization of Roseltide, a Knottin-type Neutrophil Elastase Inhibitor Derived from Hibiscus sabdariffa ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 27991569 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Loo Shining . . 2 Kam Antony . . 3 Xiao Tianshu . . 4 Nguyen Giang K. . 5 Liu 'Chuan Fa' F. . 6 Tam James P. . stop_ _Journal_abbreviation 'Sci. Rep.' _Journal_name_full 'Scientific reports' _Journal_volume 6 _Journal_issue . _Journal_ISSN 2045-2322 _Journal_CSD 0353 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 39401 _Page_last 39401 _Year 2016 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'roseltide rT1' _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 entity_1 _Molecular_mass 2629.219 _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 27 _Mol_residue_sequence ; CIPRGGICLVALSGCCNSPG CIFGICA ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 CYS 2 2 ILE 3 3 PRO 4 4 ARG 5 5 GLY 6 6 GLY 7 7 ILE 8 8 CYS 9 9 LEU 10 10 VAL 11 11 ALA 12 12 LEU 13 13 SER 14 14 GLY 15 15 CYS 16 16 CYS 17 17 ASN 18 18 SER 19 19 PRO 20 20 GLY 21 21 CYS 22 22 ILE 23 23 PHE 24 24 GLY 25 25 ILE 26 26 CYS 27 27 ALA 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 'Hibiscus sabdariffa' 183260 Eukaryota Viridiplantae Hibiscus sabdariffa 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 na . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '1.5 mM roseltide rT1, 55.6 M H2O, 2.5 M [U-2H] D2O, 1.3 mM TFA, 0.3 mM sodium chloride, 95% H2O/5% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.5 mM 'natural abundance' TFA 1.3 mM 'natural abundance' 'sodium chloride' 0.3 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_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task 'structure calculation' 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' 'peak picking' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _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' 0.3 . 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 0.000 external indirect . . . 1.0 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_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_3 stop_ 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 HA H 4.635 0.001 1 2 1 1 CYS HB2 H 3.259 0.005 . 3 1 1 CYS HB3 H 3.078 0.010 . 4 2 2 ILE H H 8.939 0.001 1 5 2 2 ILE HA H 4.476 0.005 1 6 2 2 ILE HB H 1.887 0.003 1 7 2 2 ILE HG12 H 1.043 0.001 . 8 2 2 ILE HG13 H 1.043 0.001 . 9 2 2 ILE HG2 H 1.043 0.001 1 10 2 2 ILE HD1 H 0.882 0.002 1 11 3 3 PRO HA H 4.356 0.002 1 12 3 3 PRO HB2 H 2.305 0.003 . 13 3 3 PRO HB3 H 2.010 0.003 . 14 3 3 PRO HG2 H 1.867 0.001 . 15 3 3 PRO HG3 H 1.867 0.001 . 16 3 3 PRO HD2 H 4.006 0.002 . 17 3 3 PRO HD3 H 3.810 0.003 . 18 4 4 ARG H H 8.378 0.001 1 19 4 4 ARG HA H 3.743 0.002 1 20 4 4 ARG HB2 H 1.722 0.001 . 21 4 4 ARG HB3 H 1.606 0.003 . 22 4 4 ARG HG2 H 1.478 0.002 . 23 4 4 ARG HG3 H 1.478 0.002 . 24 4 4 ARG HD2 H 3.178 0.008 . 25 4 4 ARG HD3 H 3.178 0.008 . 26 4 4 ARG HE H 7.327 0.001 1 27 5 5 GLY H H 9.256 0.001 1 28 5 5 GLY HA2 H 4.366 0.001 . 29 5 5 GLY HA3 H 3.504 0.006 . 30 6 6 GLY H H 8.453 0.001 1 31 6 6 GLY HA2 H 4.157 0.006 . 32 6 6 GLY HA3 H 3.414 0.008 . 33 7 7 ILE H H 8.107 0.001 1 34 7 7 ILE HA H 4.446 0.002 1 35 7 7 ILE HB H 1.774 0.003 1 36 7 7 ILE HG12 H 1.290 0.003 . 37 7 7 ILE HG13 H 1.290 0.003 . 38 7 7 ILE HG2 H 1.000 0.001 1 39 7 7 ILE HD1 H 0.905 0.005 1 40 8 8 CYS H H 8.396 0.002 1 41 8 8 CYS HA H 4.863 0.003 1 42 8 8 CYS HB2 H 3.182 0.008 . 43 8 8 CYS HB3 H 2.957 0.005 . 44 9 9 LEU H H 8.160 0.000 1 45 9 9 LEU HA H 4.453 0.000 1 46 9 9 LEU HB2 H 1.663 0.000 . 47 9 9 LEU HB3 H 1.663 0.000 . 48 9 9 LEU HG H 1.572 0.000 1 49 10 10 VAL H H 8.284 0.001 1 50 10 10 VAL HA H 3.728 0.001 1 51 10 10 VAL HB H 2.098 0.001 1 52 10 10 VAL HG1 H 0.926 0.006 . 53 10 10 VAL HG2 H 0.926 0.006 . 54 11 11 ALA H H 8.206 0.002 1 55 11 11 ALA HA H 4.263 0.001 1 56 11 11 ALA HB H 1.352 0.002 1 57 12 12 LEU H H 7.583 0.002 1 58 12 12 LEU HA H 4.410 0.001 1 59 12 12 LEU HB2 H 1.666 0.003 . 60 12 12 LEU HB3 H 1.579 0.003 . 61 12 12 LEU HG H 0.922 0.001 1 62 12 12 LEU HD1 H 0.872 0.005 . 63 12 12 LEU HD2 H 0.872 0.005 . 64 13 13 SER H H 8.241 0.003 1 65 13 13 SER HA H 4.345 0.001 1 66 13 13 SER HB2 H 3.999 0.004 . 67 13 13 SER HB3 H 3.898 0.002 . 68 14 14 GLY H H 8.425 0.002 1 69 14 14 GLY HA2 H 4.133 0.002 . 70 14 14 GLY HA3 H 3.968 0.005 . 71 15 15 CYS H H 8.466 0.003 1 72 15 15 CYS HA H 4.990 0.003 1 73 15 15 CYS HB2 H 3.554 0.006 . 74 15 15 CYS HB3 H 2.648 0.005 . 75 16 16 CYS H H 9.391 0.000 1 76 16 16 CYS HA H 4.355 0.003 1 77 16 16 CYS HB2 H 3.190 0.006 . 78 16 16 CYS HB3 H 2.623 0.005 . 79 17 17 ASN H H 8.540 0.001 1 80 17 17 ASN HA H 5.017 0.001 1 81 17 17 ASN HB2 H 2.823 0.007 . 82 17 17 ASN HB3 H 2.471 0.002 . 83 17 17 ASN HD21 H 7.783 0.000 . 84 17 17 ASN HD22 H 7.073 0.000 . 85 18 18 SER H H 8.613 0.002 1 86 18 18 SER HA H 4.449 0.001 1 87 18 18 SER HB2 H 3.827 0.004 . 88 18 18 SER HB3 H 3.827 0.004 . 89 19 19 PRO HA H 4.743 0.001 1 90 19 19 PRO HB2 H 2.290 0.008 . 91 19 19 PRO HB3 H 2.178 0.002 . 92 19 19 PRO HG2 H 1.951 0.004 . 93 19 19 PRO HG3 H 1.544 0.003 . 94 19 19 PRO HD2 H 3.456 0.012 . 95 19 19 PRO HD3 H 3.456 0.012 . 96 20 20 GLY H H 8.257 0.000 1 97 20 20 GLY HA2 H 4.190 0.007 . 98 20 20 GLY HA3 H 3.495 0.004 . 99 21 21 CYS H H 8.604 0.002 1 100 21 21 CYS HA H 4.529 0.003 1 101 21 21 CYS HB2 H 3.067 0.002 . 102 21 21 CYS HB3 H 2.957 0.005 . 103 22 22 ILE H H 8.740 0.001 1 104 22 22 ILE HA H 4.142 0.004 1 105 22 22 ILE HB H 1.980 0.003 1 106 22 22 ILE HG12 H 1.366 0.002 . 107 22 22 ILE HG13 H 1.174 0.002 . 108 22 22 ILE HG2 H 0.710 0.002 1 109 22 22 ILE HD1 H 0.628 0.002 1 110 23 23 PHE H H 9.009 0.001 1 111 23 23 PHE HA H 4.179 0.004 1 112 23 23 PHE HB2 H 3.452 0.010 . 113 23 23 PHE HB3 H 3.057 0.003 . 114 23 23 PHE HD1 H 7.351 0.002 . 115 23 23 PHE HD2 H 7.257 0.000 . 116 24 24 GLY H H 7.129 0.000 1 117 24 24 GLY HA2 H 4.257 0.003 . 118 24 24 GLY HA3 H 3.727 0.002 . 119 25 25 ILE H H 7.574 0.001 1 120 25 25 ILE HA H 4.901 0.002 1 121 25 25 ILE HB H 1.748 0.001 1 122 25 25 ILE HG12 H 1.433 0.001 . 123 25 25 ILE HG13 H 1.433 0.001 . 124 25 25 ILE HG2 H 1.194 0.003 1 125 25 25 ILE HD1 H 0.826 0.003 1 126 26 26 CYS H H 9.085 0.001 1 127 26 26 CYS HA H 4.823 0.002 1 128 26 26 CYS HB2 H 3.424 0.005 . 129 26 26 CYS HB3 H 2.839 0.003 . 130 27 27 ALA H H 8.822 0.001 1 131 27 27 ALA HA H 4.313 0.002 1 132 27 27 ALA HB H 1.487 0.002 1 stop_ save_