data_30619 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR Solution structure of cyclic tachyplesin I ; _BMRB_accession_number 30619 _BMRB_flat_file_name bmr30619.str _Entry_type original _Submission_date 2019-06-26 _Accession_date 2019-06-26 _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 Harvey P. J. . 2 'Troeira Henriques' S. . . 3 Vernen F. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 123 "13C chemical shifts" 52 "15N chemical shifts" 16 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-09-05 original BMRB . stop_ _Original_release_date 2019-08-02 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Characterization of Tachyplesin Peptides and Their Cyclized Analogues to Improve Antimicrobial and Anticancer Properties ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 31455019 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Vernen Felicitas . . 2 Harvey Peta J. . 3 Dias Susana A. . 4 Veiga 'Ana Salome' S. . 5 Huang Yen-Hua H. . 6 Craik David J. . 7 Lawrence Nicole . . 8 'Troeira Henriques' Sonia . . stop_ _Journal_abbreviation 'Int. J. Mol. Sci.' _Journal_name_full 'International journal of molecular sciences' _Journal_volume 20 _Journal_issue 17 _Journal_ISSN 1422-0067 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first E4184 _Page_last E4184 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Tachyplesin-1 _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 2331.858 _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 18 _Mol_residue_sequence ; KWCFRVCYRGICYRRCRG ; loop_ _Residue_seq_code _Residue_label 1 LYS 2 TRP 3 CYS 4 PHE 5 ARG 6 VAL 7 CYS 8 TYR 9 ARG 10 GLY 11 ILE 12 CYS 13 TYR 14 ARG 15 ARG 16 CYS 17 ARG 18 GLY 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 'Japanese horseshoe crab' 6853 Eukaryota Metazoa Tachypleus tridentatus 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 'lyophilized powder' _Details '1.0 mg/mL cyclic tachyplesin I, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.0 mg/mL 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type 'lyophilized powder' _Details '1.0 mg/mL cyclic tachyplesin I, 100% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.0 mg/mL 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name TopSpin _Version 3.6.1 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task processing stop_ _Details . save_ save_software_2 _Saveframe_category software _Name 'CcpNmr Analysis' _Version . loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_software_3 _Saveframe_category software _Name CYANA _Version . loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure calculation' stop_ _Details . save_ save_software_4 _Saveframe_category software _Name CNS _Version . loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task refinement stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model 'AVANCE III' _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_ save_2D_E.COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D E.COSY' _Sample_label $sample_2 save_ save_2D_1H-15N_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_2 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 4 . 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 C 13 'methyl protons' ppm 0.000 internal indirect . . . 0.25144953 DSS H 1 'methyl protons' ppm 0.000 internal direct . . . 1.0 DSS N 15 'methyl protons' ppm 0.000 internal indirect . . . 0.10132912 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' '2D E.COSY' '2D 1H-15N HSQC' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 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 LYS H H 8.703 0.002 1 2 1 1 LYS HA H 4.187 0.007 1 3 1 1 LYS HB2 H 1.750 0.007 2 4 1 1 LYS HB3 H 1.534 0.007 2 5 1 1 LYS HG2 H 1.215 0.008 2 6 1 1 LYS HG3 H 1.108 0.009 2 7 1 1 LYS HD2 H 1.535 0.009 2 8 1 1 LYS HD3 H 1.535 0.009 2 9 1 1 LYS HE2 H 2.852 0.008 2 10 1 1 LYS HE3 H 2.852 0.008 2 11 1 1 LYS HZ H 7.475 0.001 1 12 1 1 LYS CA C 56.449 0.000 1 13 1 1 LYS CB C 32.145 0.012 1 14 1 1 LYS CG C 24.364 0.012 1 15 1 1 LYS CD C 28.895 0.000 1 16 1 1 LYS CE C 41.717 0.000 1 17 1 1 LYS N N 121.573 0.000 1 18 2 2 TRP H H 7.826 0.004 1 19 2 2 TRP HA H 4.913 0.009 1 20 2 2 TRP HB2 H 3.508 0.009 2 21 2 2 TRP HB3 H 3.266 0.006 2 22 2 2 TRP HD1 H 7.320 0.001 1 23 2 2 TRP HE1 H 10.135 0.004 1 24 2 2 TRP HE3 H 7.757 0.004 1 25 2 2 TRP HZ2 H 7.398 0.004 1 26 2 2 TRP HH2 H 7.100 0.003 1 27 2 2 TRP CA C 56.309 0.000 1 28 2 2 TRP CB C 29.864 0.012 1 29 2 2 TRP N N 122.618 0.000 1 30 2 2 TRP NE1 N 129.038 0.000 1 31 3 3 CYS H H 8.359 0.003 1 32 3 3 CYS HA H 5.395 0.013 1 33 3 3 CYS HB2 H 2.912 0.013 2 34 3 3 CYS HB3 H 2.473 0.008 2 35 3 3 CYS CA C 55.365 0.000 1 36 3 3 CYS CB C 47.854 0.007 1 37 3 3 CYS N N 123.700 0.000 1 38 4 4 PHE H H 8.727 0.008 1 39 4 4 PHE HA H 4.790 0.013 1 40 4 4 PHE HB2 H 2.930 0.007 2 41 4 4 PHE HB3 H 2.926 0.003 2 42 4 4 PHE HD1 H 6.691 0.002 3 43 4 4 PHE HD2 H 6.691 0.002 3 44 4 4 PHE HE1 H 6.995 0.002 3 45 4 4 PHE HE2 H 6.995 0.002 3 46 4 4 PHE CA C 55.628 0.000 1 47 4 4 PHE CB C 40.839 0.000 1 48 4 4 PHE N N 127.686 0.000 1 49 5 5 ARG H H 8.586 0.001 1 50 5 5 ARG HA H 4.956 0.008 1 51 5 5 ARG HB2 H 1.699 0.014 2 52 5 5 ARG HB3 H 1.625 0.008 2 53 5 5 ARG HG2 H 1.486 0.008 2 54 5 5 ARG HG3 H 1.405 0.008 2 55 5 5 ARG HD2 H 3.092 0.010 2 56 5 5 ARG HD3 H 3.094 0.009 2 57 5 5 ARG HE H 7.173 0.003 1 58 5 5 ARG CA C 55.125 0.000 1 59 5 5 ARG CB C 32.165 0.003 1 60 5 5 ARG CG C 27.898 0.004 1 61 5 5 ARG CD C 43.781 0.000 1 62 5 5 ARG N N 123.915 0.000 1 63 6 6 VAL H H 8.882 0.004 1 64 6 6 VAL HA H 4.348 0.009 1 65 6 6 VAL HB H 1.681 0.014 1 66 6 6 VAL HG1 H 0.882 0.008 . 67 6 6 VAL HG2 H 0.882 0.009 . 68 6 6 VAL CA C 60.864 0.000 1 69 6 6 VAL CB C 34.477 0.000 1 70 6 6 VAL CG1 C 20.919 0.000 2 71 6 6 VAL CG2 C 20.919 0.000 2 72 6 6 VAL N N 126.206 0.000 1 73 7 7 CYS H H 8.656 0.002 1 74 7 7 CYS HA H 5.614 0.007 1 75 7 7 CYS HB2 H 3.018 0.006 2 76 7 7 CYS HB3 H 2.635 0.009 2 77 7 7 CYS CA C 55.184 0.000 1 78 7 7 CYS CB C 48.591 0.004 1 79 7 7 CYS N N 122.049 0.000 1 80 8 8 TYR H H 9.107 0.002 1 81 8 8 TYR HA H 4.718 0.010 1 82 8 8 TYR HB2 H 3.023 0.009 2 83 8 8 TYR HB3 H 3.025 0.012 2 84 8 8 TYR HD1 H 6.817 0.003 3 85 8 8 TYR HD2 H 6.817 0.003 3 86 8 8 TYR HE1 H 7.213 0.008 3 87 8 8 TYR HE2 H 7.213 0.008 3 88 8 8 TYR CA C 57.511 0.000 1 89 8 8 TYR CB C 40.692 0.000 1 90 8 8 TYR N N 123.566 0.000 1 91 9 9 ARG H H 9.250 0.001 1 92 9 9 ARG HA H 3.694 0.006 1 93 9 9 ARG HB2 H 1.903 0.008 2 94 9 9 ARG HB3 H 1.592 0.009 2 95 9 9 ARG HG2 H 1.225 0.010 2 96 9 9 ARG HG3 H 0.922 0.010 2 97 9 9 ARG HD2 H 3.042 0.008 2 98 9 9 ARG HD3 H 3.042 0.008 2 99 9 9 ARG HE H 7.015 0.002 1 100 9 9 ARG CA C 57.085 0.000 1 101 9 9 ARG CB C 27.910 0.003 1 102 9 9 ARG CG C 27.310 0.016 1 103 9 9 ARG CD C 43.540 0.000 1 104 9 9 ARG N N 125.530 0.000 1 105 10 10 GLY H H 8.554 0.005 1 106 10 10 GLY HA2 H 4.137 0.007 2 107 10 10 GLY HA3 H 3.541 0.013 2 108 10 10 GLY CA C 45.169 0.025 1 109 11 11 ILE H H 7.773 0.004 1 110 11 11 ILE HA H 4.288 0.006 1 111 11 11 ILE HB H 1.991 0.007 1 112 11 11 ILE HG12 H 1.493 0.009 2 113 11 11 ILE HG13 H 1.152 0.007 2 114 11 11 ILE HG2 H 0.760 0.005 . 115 11 11 ILE HD1 H 0.864 0.005 . 116 11 11 ILE CA C 59.965 0.000 1 117 11 11 ILE CB C 38.876 0.000 1 118 11 11 ILE CG1 C 27.039 0.026 1 119 11 11 ILE CG2 C 17.294 0.000 1 120 11 11 ILE CD1 C 12.077 0.000 1 121 12 12 CYS H H 8.569 0.002 1 122 12 12 CYS HA H 5.681 0.010 1 123 12 12 CYS HB2 H 2.923 0.007 2 124 12 12 CYS HB3 H 2.522 0.007 2 125 12 12 CYS CA C 55.061 0.000 1 126 12 12 CYS CB C 47.647 0.015 1 127 12 12 CYS N N 123.897 0.000 1 128 13 13 TYR H H 9.160 0.003 1 129 13 13 TYR HA H 4.735 0.016 1 130 13 13 TYR HB2 H 3.038 0.012 2 131 13 13 TYR HB3 H 2.834 0.008 2 132 13 13 TYR HD1 H 6.707 0.005 3 133 13 13 TYR HD2 H 6.707 0.005 3 134 13 13 TYR HE1 H 7.008 0.003 3 135 13 13 TYR HE2 H 7.008 0.003 3 136 13 13 TYR CA C 56.168 0.000 1 137 13 13 TYR CB C 40.857 0.003 1 138 13 13 TYR N N 123.545 0.000 1 139 14 14 ARG H H 8.651 0.002 1 140 14 14 ARG HA H 4.803 0.015 1 141 14 14 ARG HB2 H 1.695 0.007 2 142 14 14 ARG HB3 H 1.580 0.006 2 143 14 14 ARG HG2 H 1.407 0.005 2 144 14 14 ARG HG3 H 1.307 0.007 2 145 14 14 ARG HD2 H 3.072 0.008 2 146 14 14 ARG HD3 H 3.072 0.008 2 147 14 14 ARG HE H 7.160 0.000 1 148 14 14 ARG CA C 55.177 0.000 1 149 14 14 ARG CB C 31.505 0.001 1 150 14 14 ARG CG C 27.929 0.003 1 151 14 14 ARG CD C 43.552 0.000 1 152 14 14 ARG N N 121.953 0.000 1 153 15 15 ARG H H 8.712 0.002 1 154 15 15 ARG HA H 4.522 0.005 1 155 15 15 ARG HB2 H 1.417 0.008 2 156 15 15 ARG HB3 H 1.254 0.007 2 157 15 15 ARG HG2 H 1.531 0.011 2 158 15 15 ARG HG3 H 1.411 0.014 2 159 15 15 ARG HD2 H 3.209 0.007 2 160 15 15 ARG HD3 H 3.121 0.008 2 161 15 15 ARG HE H 7.145 0.004 1 162 15 15 ARG CA C 54.193 0.000 1 163 15 15 ARG CB C 33.265 0.007 1 164 15 15 ARG CG C 27.058 0.011 1 165 15 15 ARG CD C 43.248 0.003 1 166 15 15 ARG N N 127.686 0.000 1 167 16 16 CYS H H 8.603 0.002 1 168 16 16 CYS HA H 5.392 0.009 1 169 16 16 CYS HB2 H 2.900 0.011 2 170 16 16 CYS HB3 H 2.900 0.011 2 171 16 16 CYS CA C 55.731 0.000 1 172 16 16 CYS CB C 48.295 0.000 1 173 16 16 CYS N N 121.337 0.000 1 174 17 17 ARG H H 9.201 0.004 1 175 17 17 ARG HA H 4.564 0.006 1 176 17 17 ARG HB2 H 2.071 0.007 2 177 17 17 ARG HB3 H 1.944 0.005 2 178 17 17 ARG HG2 H 1.762 0.006 2 179 17 17 ARG HG3 H 1.677 0.006 2 180 17 17 ARG HD2 H 3.305 0.007 2 181 17 17 ARG HD3 H 3.305 0.007 2 182 17 17 ARG HE H 7.293 0.001 1 183 17 17 ARG CA C 55.201 0.000 1 184 17 17 ARG CB C 31.218 0.006 1 185 17 17 ARG CG C 27.199 0.006 1 186 17 17 ARG CD C 43.555 0.000 1 187 17 17 ARG N N 121.031 0.000 1 188 18 18 GLY H H 8.948 0.002 1 189 18 18 GLY HA2 H 4.073 0.007 2 190 18 18 GLY HA3 H 3.643 0.005 2 191 18 18 GLY CA C 46.606 0.016 1 stop_ save_